# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Zn3Cl6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H42 Cl6 N6 O6 Zn3' _chemical_formula_weight 1027.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 32.1306(4) _cell_length_b 32.1306(4) _cell_length_c 7.38800(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6605.34(15) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9968 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 21.35 _exptl_crystal_description BLOCK _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3132 _exptl_absorpt_coefficient_mu 2.032 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4617 _exptl_absorpt_correction_T_max 0.6306 _exptl_absorpt_process_details sadabs _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 'Bruker Breeze CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 122516 _diffrn_reflns_av_R_equivalents 0.0824 _diffrn_reflns_av_unetI/netI 0.0457 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 0.73 _diffrn_reflns_theta_max 28.32 _reflns_number_total 10940 _reflns_number_gt 9034 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0548P)^2^+0.5374P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.016(10) _refine_ls_number_reflns 10940 _refine_ls_number_parameters 515 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.0997 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 -0.525972(16) -0.901215(15) -0.51809(7) 0.03271(11) Uani 1 1 d . . . Zn2 Zn -0.43087(7) -0.28361(4) -0.48375(13) 0.0350(3) Uani 0.817(5) 1 d P A 1 Zn2' Zn -0.4083(3) -0.27529(15) -0.5052(5) 0.0306(11) Uani 0.183(5) 1 d P A 2 Zn3 Zn -0.243914(15) -0.078860(16) -1.20263(7) 0.02904(10) Uani 1 1 d . . . Cl1 Cl -0.60289(4) -0.94906(4) -0.46331(17) 0.0499(3) Uani 1 1 d . . . Cl2 Cl -0.47817(4) -0.85816(4) -0.29081(15) 0.0463(3) Uani 1 1 d . . . Cl3 Cl -0.48391(8) -0.28657(6) -0.28293(19) 0.0421(5) Uani 0.817(5) 1 d P A 1 Cl4 Cl -0.38117(10) -0.30828(9) -0.4094(3) 0.0692(8) Uani 0.817(5) 1 d P A 1 Cl3' Cl -0.4673(3) -0.2973(3) -0.3062(9) 0.042(2) Uani 0.183(5) 1 d P A 2 Cl4' Cl -0.3457(4) -0.2816(3) -0.4334(10) 0.050(3) Uani 0.183(5) 1 d P A 2 Cl5 Cl -0.30028(4) -0.06150(4) -1.26476(18) 0.0497(3) Uani 1 1 d . . . Cl6 Cl -0.18973(4) -0.06964(4) -1.40995(13) 0.0376(2) Uani 1 1 d . . . O1 O -0.44035(9) -0.77917(9) -0.7296(4) 0.0312(6) Uani 1 1 d . . . O2 O -0.52491(9) -0.85287(10) -0.6889(4) 0.0418(7) Uani 1 1 d . . . H2C H -0.4979 -0.8319 -0.7278 0.050 Uiso 1 1 d R . . O3 O -0.55344(9) -0.32632(9) -0.7227(4) 0.0347(6) Uani 1 1 d . . . O4 O -0.47425(13) -0.32862(14) -0.6777(5) 0.0599(9) Uani 1 1 d . . . H4C H -0.5092 -0.3432 -0.6666 0.072 Uiso 1 1 d R A . O5 O -0.12028(8) -0.02306(9) -0.9677(3) 0.0280(6) Uani 1 1 d . . . O6 O -0.20485(9) -0.03131(10) -1.0079(4) 0.0418(7) Uani 1 1 d . . . H6D H -0.1768 -0.0254 -0.9842 0.050 Uiso 1 1 d R . . N1 N -0.49753(12) -0.93915(11) -0.6401(4) 0.0328(8) Uani 1 1 d . . . N2 N -0.39435(11) -0.79871(10) -0.9019(4) 0.0283(7) Uani 1 1 d . . . H2B H -0.3690 -0.7876 -0.9727 0.034 Uiso 1 1 calc R . . N3 N -0.39146(12) -0.21397(13) -0.5989(4) 0.0368(8) Uani 1 1 d . . . N4 N -0.53462(11) -0.26212(11) -0.9026(5) 0.0303(7) Uani 1 1 d . . . H4B H -0.5458 -0.2483 -0.9753 0.036 Uiso 1 1 calc R . . N5 N -0.27506(10) -0.14639(11) -1.0914(4) 0.0263(7) Uani 1 1 d . . . N6 N -0.13013(10) -0.08612(10) -0.7970(4) 0.0245(6) Uani 1 1 d . . . H6C H -0.1157 -0.0975 -0.7286 0.029 Uiso 1 1 calc R . . C1 C -0.52710(18) -0.98743(14) -0.6417(6) 0.0413(10) Uani 1 1 d . . . H1A H -0.5604 -1.0000 -0.6204 0.050 Uiso 1 1 calc R . . C2 C -0.51063(19) -1.01922(15) -0.6731(6) 0.0447(11) Uani 1 1 d . . . H2A H -0.5321 -1.0529 -0.6745 0.054 Uiso 1 1 calc R . . C3 C -0.46230(18) -1.00054(15) -0.7019(6) 0.0460(11) Uani 1 1 d . . . H3A H -0.4495 -1.0213 -0.7168 0.055 Uiso 1 1 calc R . . C4 C -0.43254(16) -0.95131(14) -0.7091(6) 0.0399(9) Uani 1 1 d . . . H4A H -0.3994 -0.9381 -0.7357 0.048 Uiso 1 1 calc R . . C5 C -0.45103(14) -0.92131(13) -0.6776(5) 0.0291(8) Uani 1 1 d . . . C6 C -0.41968(14) -0.86741(13) -0.6910(6) 0.0327(8) Uani 1 1 d . . . H6A H -0.3858 -0.8581 -0.6680 0.039 Uiso 1 1 calc R . . H6B H -0.4296 -0.8518 -0.5984 0.039 Uiso 1 1 calc R . . C7 C -0.42434(14) -0.85043(12) -0.8807(5) 0.0273(8) Uani 1 1 d . . . H7A H -0.4151 -0.8667 -0.9725 0.033 Uiso 1 1 calc R . . H7B H -0.4583 -0.8597 -0.9023 0.033 Uiso 1 1 calc R . . C8 C -0.40332(13) -0.76772(12) -0.8203(5) 0.0237(7) Uani 1 1 d . . . C9 C -0.36641(12) -0.71535(12) -0.8354(4) 0.0218(7) Uani 1 1 d . . . C10 C -0.38240(13) -0.68232(13) -0.8355(4) 0.0222(7) Uani 1 1 d . . . H10 H -0.4158 -0.6930 -0.8355 0.027 Uiso 1 1 calc R . . C11 C -0.56185(16) -0.85627(18) -0.8042(7) 0.0557(13) Uani 1 1 d . . . H11A H -0.5502 -0.8261 -0.8709 0.067 Uiso 1 1 calc R . . H11B H -0.5898 -0.8624 -0.7313 0.067 Uiso 1 1 calc R . . H11C H -0.5711 -0.8827 -0.8900 0.067 Uiso 1 1 calc R . . C12 C -0.34393(17) -0.1914(2) -0.5820(6) 0.0532(13) Uani 1 1 d . A . H12A H -0.3294 -0.2080 -0.5294 0.064 Uiso 1 1 calc R B 2 C13 C -0.31494(19) -0.1445(3) -0.6385(8) 0.075(2) Uani 1 1 d . . . H13A H -0.2811 -0.1289 -0.6227 0.091 Uiso 1 1 calc R A . C14 C -0.33605(19) -0.12090(19) -0.7182(8) 0.0679(17) Uani 1 1 d . A . H14A H -0.3170 -0.0887 -0.7587 0.081 Uiso 1 1 calc R . . C15 C -0.38583(16) -0.14518(17) -0.7382(6) 0.0468(11) Uani 1 1 d . . . H15A H -0.4011 -0.1297 -0.7943 0.056 Uiso 1 1 calc R A . C16 C -0.41268(13) -0.19149(14) -0.6765(5) 0.0305(8) Uani 1 1 d . A . C17 C -0.46640(13) -0.21796(14) -0.6929(6) 0.0332(8) Uani 1 1 d . . . H17A H -0.4785 -0.1955 -0.6700 0.040 Uiso 1 1 calc R A . H17B H -0.4804 -0.2436 -0.6003 0.040 Uiso 1 1 calc R . . C18 C -0.48255(13) -0.24023(14) -0.8812(5) 0.0321(9) Uani 1 1 d . A . H18A H -0.4661 -0.2150 -0.9743 0.039 Uiso 1 1 calc R . . H18B H -0.4732 -0.2650 -0.8995 0.039 Uiso 1 1 calc R . . C19 C -0.56550(13) -0.30195(13) -0.8168(5) 0.0262(8) Uani 1 1 d . . . C20 C -0.61738(12) -0.31719(13) -0.8346(5) 0.0248(7) Uani 1 1 d . . . C21 C -0.65121(12) -0.36690(12) -0.8323(4) 0.0224(7) Uani 1 1 d . . . H21 H -0.6405 -0.3896 -0.8292 0.027 Uiso 1 1 calc R . . C22 C -0.4637(2) -0.3531(2) -0.8096(8) 0.0652(15) Uani 1 1 d . A . H22A H -0.4924 -0.3729 -0.8823 0.078 Uiso 1 1 calc R . . H22B H -0.4532 -0.3737 -0.7510 0.078 Uiso 1 1 calc R . . H22C H -0.4379 -0.3298 -0.8880 0.078 Uiso 1 1 calc R . . C23 C -0.25092(13) -0.16692(13) -1.0183(5) 0.0291(8) Uani 1 1 d . . . C24 C -0.27569(15) -0.21396(15) -0.9547(6) 0.0393(10) Uani 1 1 d . . . H24A H -0.2588 -0.2279 -0.9000 0.047 Uiso 1 1 calc R . . C25 C -0.32580(16) -0.24065(15) -0.9720(7) 0.0487(12) Uani 1 1 d . . . H25A H -0.3432 -0.2731 -0.9321 0.058 Uiso 1 1 calc R . . C26 C -0.34916(15) -0.21935(15) -1.0471(6) 0.0409(10) Uani 1 1 d . . . H26A H -0.3831 -0.2367 -1.0595 0.049 Uiso 1 1 calc R . . C27 C -0.32335(14) -0.17301(15) -1.1041(5) 0.0348(9) Uani 1 1 d . . . H27A H -0.3402 -0.1586 -1.1556 0.042 Uiso 1 1 calc R . . C28 C -0.19772(12) -0.13766(13) -1.0020(5) 0.0281(7) Uani 1 1 d . . . H28A H -0.1852 -0.1124 -1.0964 0.034 Uiso 1 1 calc R . . H28B H -0.1836 -0.1585 -1.0230 0.034 Uiso 1 1 calc R . . C29 C -0.18209(12) -0.11395(13) -0.8147(5) 0.0265(8) Uani 1 1 d . . . H29A H -0.1957 -0.0926 -0.7948 0.032 Uiso 1 1 calc R . . H29B H -0.1952 -0.1392 -0.7203 0.032 Uiso 1 1 calc R . . C30 C -0.10351(12) -0.04418(12) -0.8799(4) 0.0217(7) Uani 1 1 d . . . C31 C -0.04981(11) -0.02212(12) -0.8660(4) 0.0194(7) Uani 1 1 d . . . C32 C -0.02832(12) -0.05015(12) -0.8666(4) 0.0204(7) Uani 1 1 d . . . H32 H -0.0474 -0.0842 -0.8675 0.024 Uiso 1 1 calc R . . C33 C -0.21587(17) -0.00136(17) -0.8995(7) 0.0492(12) Uani 1 1 d . . . H33A H -0.1895 0.0170 -0.8147 0.059 Uiso 1 1 calc R . . H33B H -0.2455 -0.0214 -0.8316 0.059 Uiso 1 1 calc R . . H33C H -0.2202 0.0208 -0.9777 0.059 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 0.0371(2) 0.0267(2) 0.0307(2) 0.00112(19) -0.0006(2) 0.0132(2) Zn2 0.0407(7) 0.0415(5) 0.0298(4) -0.0043(3) -0.0064(4) 0.0259(5) Zn2' 0.030(3) 0.0361(16) 0.0236(14) -0.0012(12) 0.0017(16) 0.0149(18) Zn3 0.0257(2) 0.0328(2) 0.0292(2) -0.0030(2) -0.00333(19) 0.01501(19) Cl1 0.0416(6) 0.0391(6) 0.0559(7) 0.0111(5) 0.0096(5) 0.0104(5) Cl2 0.0659(7) 0.0477(6) 0.0323(5) -0.0117(5) -0.0143(5) 0.0336(6) Cl3 0.0509(10) 0.0442(8) 0.0295(6) -0.0007(6) 0.0053(6) 0.0224(7) Cl4 0.0733(18) 0.0736(15) 0.0850(13) -0.0196(11) -0.0355(12) 0.0549(15) Cl3' 0.038(4) 0.059(4) 0.031(3) 0.006(3) 0.008(3) 0.026(3) Cl4' 0.064(7) 0.052(5) 0.054(4) 0.002(3) -0.005(3) 0.043(5) Cl5 0.0350(6) 0.0516(7) 0.0688(8) -0.0037(6) -0.0158(5) 0.0265(5) Cl6 0.0363(5) 0.0417(6) 0.0301(5) -0.0015(4) 0.0049(4) 0.0161(5) O1 0.0272(13) 0.0249(13) 0.0344(15) 0.0001(11) 0.0054(11) 0.0077(11) O2 0.0252(14) 0.0365(16) 0.0489(17) 0.0141(14) -0.0051(14) 0.0044(12) O3 0.0282(14) 0.0331(14) 0.0452(17) 0.0107(13) 0.0006(13) 0.0171(12) O4 0.053(2) 0.084(3) 0.057(2) -0.022(2) -0.0141(17) 0.044(2) O5 0.0202(12) 0.0273(13) 0.0354(15) 0.0066(11) -0.0009(11) 0.0111(11) O6 0.0298(14) 0.0526(17) 0.0528(18) -0.0278(15) -0.0189(14) 0.0279(14) N1 0.042(2) 0.0215(16) 0.0286(16) -0.0039(13) -0.0052(14) 0.0107(15) N2 0.0282(17) 0.0216(15) 0.0292(16) -0.0001(13) 0.0068(13) 0.0081(13) N3 0.038(2) 0.054(2) 0.0268(17) -0.0081(15) -0.0038(15) 0.0289(18) N4 0.0209(15) 0.0338(18) 0.0332(16) 0.0076(14) 0.0017(13) 0.0114(14) N5 0.0190(15) 0.0285(16) 0.0258(15) -0.0055(13) 0.0002(12) 0.0077(13) N6 0.0203(15) 0.0236(15) 0.0287(15) 0.0051(13) 0.0002(12) 0.0103(13) C1 0.050(3) 0.022(2) 0.040(2) -0.0036(17) 0.0031(19) 0.0092(19) C2 0.071(3) 0.030(2) 0.029(2) 0.0020(17) 0.002(2) 0.022(2) C3 0.072(3) 0.034(2) 0.041(2) -0.007(2) -0.010(2) 0.032(2) C4 0.048(2) 0.036(2) 0.039(2) -0.001(2) -0.002(2) 0.024(2) C5 0.039(2) 0.0279(19) 0.0201(18) -0.0019(14) -0.0040(16) 0.0164(17) C6 0.033(2) 0.0229(18) 0.037(2) 0.0015(17) -0.0087(18) 0.0105(16) C7 0.0297(19) 0.0223(18) 0.0259(18) -0.0003(14) 0.0009(15) 0.0099(16) C8 0.0251(18) 0.0256(18) 0.0224(18) 0.0037(14) -0.0001(14) 0.0141(16) C9 0.0266(18) 0.0184(17) 0.0177(16) 0.0001(13) 0.0022(13) 0.0093(15) C10 0.0247(18) 0.0270(18) 0.0166(15) -0.0018(13) -0.0003(13) 0.0142(15) C11 0.039(3) 0.054(3) 0.060(3) 0.012(3) -0.020(2) 0.013(2) C12 0.037(3) 0.094(4) 0.034(2) -0.023(3) -0.008(2) 0.037(3) C13 0.029(3) 0.121(6) 0.053(3) -0.046(4) -0.009(2) 0.019(3) C14 0.048(3) 0.050(3) 0.062(3) -0.017(3) 0.016(3) -0.008(3) C15 0.046(3) 0.043(3) 0.043(3) 0.005(2) 0.007(2) 0.015(2) C16 0.0256(19) 0.034(2) 0.0254(19) -0.0053(16) 0.0026(15) 0.0104(16) C17 0.0247(18) 0.036(2) 0.034(2) -0.0016(18) 0.0019(17) 0.0121(17) C18 0.0240(19) 0.035(2) 0.031(2) 0.0042(17) 0.0021(15) 0.0104(17) C19 0.0270(19) 0.0265(19) 0.0236(18) -0.0024(14) -0.0004(14) 0.0123(16) C20 0.0217(18) 0.032(2) 0.0213(16) 0.0021(14) 0.0021(13) 0.0136(16) C21 0.0237(18) 0.0224(17) 0.0216(17) 0.0030(13) 0.0021(13) 0.0120(15) C22 0.078(4) 0.064(3) 0.074(4) -0.020(3) -0.011(3) 0.051(3) C23 0.0278(18) 0.0287(18) 0.0282(18) -0.0055(16) -0.0037(16) 0.0122(16) C24 0.034(2) 0.035(2) 0.047(2) -0.0031(18) 0.0012(18) 0.0158(19) C25 0.043(3) 0.028(2) 0.056(3) -0.007(2) 0.005(2) 0.0039(19) C26 0.025(2) 0.040(2) 0.041(2) -0.0066(19) 0.0020(17) 0.0029(18) C27 0.024(2) 0.043(2) 0.031(2) -0.0088(18) -0.0032(16) 0.0124(18) C28 0.0262(18) 0.0317(19) 0.0274(18) 0.0007(16) 0.0017(16) 0.0153(15) C29 0.0207(17) 0.0264(19) 0.0273(19) 0.0013(15) 0.0012(14) 0.0078(15) C30 0.0210(17) 0.0250(18) 0.0204(17) -0.0026(14) -0.0008(13) 0.0125(15) C31 0.0197(17) 0.0242(17) 0.0141(15) 0.0008(13) -0.0004(12) 0.0108(14) C32 0.0202(17) 0.0236(17) 0.0190(16) -0.0018(13) -0.0026(13) 0.0121(15) C33 0.047(3) 0.051(3) 0.045(3) -0.017(2) -0.003(2) 0.022(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 O2 1.988(3) . ? Zn1 N1 2.061(3) . ? Zn1 Cl1 2.1991(12) . ? Zn1 Cl2 2.2289(11) . ? Zn2 O4 2.018(4) . ? Zn2 N3 2.121(4) . ? Zn2 Cl4 2.1788(18) . ? Zn2 Cl3 2.2253(18) . ? Zn2' N3 1.894(5) . ? Zn2' Cl4' 2.184(8) . ? Zn2' Cl3' 2.216(7) . ? Zn2' O4 2.328(7) . ? Zn2' C12 2.509(8) . ? Zn3 O6 2.015(3) . ? Zn3 N5 2.053(3) . ? Zn3 Cl5 2.1937(11) . ? Zn3 Cl6 2.2246(11) . ? O1 C8 1.250(4) . ? O2 C11 1.420(5) . ? O2 H2C 0.8401 . ? O3 C19 1.245(4) . ? O4 C22 1.396(6) . ? O4 H4C 0.9798 . ? O5 C30 1.240(4) . ? O6 C33 1.426(5) . ? O6 H6D 0.8399 . ? N1 C5 1.334(5) . ? N1 C1 1.355(5) . ? N2 C8 1.313(5) . ? N2 C7 1.454(4) . ? N2 H2B 0.8800 . ? N3 C12 1.329(6) . ? N3 C16 1.345(5) . ? N4 C19 1.324(5) . ? N4 C18 1.464(5) . ? N4 H4B 0.8800 . ? N5 C27 1.349(5) . ? N5 C23 1.356(5) . ? N6 C30 1.330(4) . ? N6 C29 1.453(4) . ? N6 H6C 0.8800 . ? C1 C2 1.385(6) . ? C1 H1A 0.9500 . ? C2 C3 1.373(7) . ? C2 H2A 0.9500 . ? C3 C4 1.381(6) . ? C3 H3A 0.9500 . ? C4 C5 1.382(6) . ? C4 H4A 0.9500 . ? C5 C6 1.510(5) . ? C6 C7 1.538(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.502(5) . ? C9 C10 1.387(5) 2_445 ? C9 C10 1.391(5) . ? C10 C9 1.387(5) 3_545 ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.380(9) . ? C12 H12A 0.9500 . ? C13 C14 1.377(9) . ? C13 H13A 0.9500 . ? C14 C15 1.393(7) . ? C14 H14A 0.9500 . ? C15 C16 1.372(6) . ? C15 H15A 0.9500 . ? C16 C17 1.500(5) . ? C17 C18 1.531(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.490(5) . ? C20 C21 1.380(5) 2_455 ? C20 C21 1.413(5) . ? C21 C20 1.380(5) 3_445 ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.391(6) . ? C23 C28 1.488(5) . ? C24 C25 1.401(6) . ? C24 H24A 0.9500 . ? C25 C26 1.361(7) . ? C25 H25A 0.9500 . ? C26 C27 1.359(6) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 C29 1.538(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.506(5) . ? C31 C32 1.382(5) . ? C31 C32 1.406(5) 3 ? C32 C31 1.407(5) 2 ? C32 H32 0.9500 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 N1 110.17(13) . . ? O2 Zn1 Cl1 103.72(8) . . ? N1 Zn1 Cl1 110.05(10) . . ? O2 Zn1 Cl2 104.83(9) . . ? N1 Zn1 Cl2 108.96(10) . . ? Cl1 Zn1 Cl2 118.69(5) . . ? O4 Zn2 N3 107.78(15) . . ? O4 Zn2 Cl4 106.72(12) . . ? N3 Zn2 Cl4 108.98(12) . . ? O4 Zn2 Cl3 101.72(13) . . ? N3 Zn2 Cl3 110.66(10) . . ? Cl4 Zn2 Cl3 120.09(9) . . ? N3 Zn2' Cl4' 112.8(3) . . ? N3 Zn2' Cl3' 109.1(3) . . ? Cl4' Zn2' Cl3' 119.3(3) . . ? N3 Zn2' O4 104.3(3) . . ? Cl4' Zn2' O4 127.3(3) . . ? Cl3' Zn2' O4 79.1(3) . . ? N3 Zn2' C12 31.36(18) . . ? Cl4' Zn2' C12 81.5(3) . . ? Cl3' Zn2' C12 127.3(3) . . ? O4 Zn2' C12 128.7(2) . . ? O6 Zn3 N5 107.77(13) . . ? O6 Zn3 Cl5 103.71(8) . . ? N5 Zn3 Cl5 108.93(9) . . ? O6 Zn3 Cl6 103.96(9) . . ? N5 Zn3 Cl6 110.61(9) . . ? Cl5 Zn3 Cl6 120.84(5) . . ? C11 O2 Zn1 129.3(3) . . ? C11 O2 H2C 110.2 . . ? Zn1 O2 H2C 116.9 . . ? C22 O4 Zn2 128.6(3) . . ? C22 O4 Zn2' 114.1(4) . . ? Zn2 O4 Zn2' 15.29(13) . . ? C22 O4 H4C 109.4 . . ? Zn2 O4 H4C 119.9 . . ? Zn2' O4 H4C 135.2 . . ? C33 O6 Zn3 129.9(2) . . ? C33 O6 H6D 109.2 . . ? Zn3 O6 H6D 120.7 . . ? C5 N1 C1 118.9(4) . . ? C5 N1 Zn1 124.7(2) . . ? C1 N1 Zn1 114.6(3) . . ? C8 N2 C7 123.1(3) . . ? C8 N2 H2B 118.5 . . ? C7 N2 H2B 118.5 . . ? C12 N3 C16 119.9(4) . . ? C12 N3 Zn2' 100.8(4) . . ? C16 N3 Zn2' 139.2(4) . . ? C12 N3 Zn2 117.1(3) . . ? C16 N3 Zn2 122.8(3) . . ? Zn2' N3 Zn2 17.6(2) . . ? C19 N4 C18 122.5(3) . . ? C19 N4 H4B 118.8 . . ? C18 N4 H4B 118.8 . . ? C27 N5 C23 118.4(3) . . ? C27 N5 Zn3 116.1(3) . . ? C23 N5 Zn3 125.3(2) . . ? C30 N6 C29 122.7(3) . . ? C30 N6 H6C 118.6 . . ? C29 N6 H6C 118.6 . . ? N1 C1 C2 122.6(5) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 118.0(4) . . ? C3 C2 H2A 121.0 . . ? C1 C2 H2A 121.0 . . ? C2 C3 C4 119.4(4) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C3 C4 C5 120.0(4) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? N1 C5 C4 121.0(4) . . ? N1 C5 C6 117.9(3) . . ? C4 C5 C6 121.1(4) . . ? C5 C6 C7 109.8(3) . . ? C5 C6 H6A 109.7 . . ? C7 C6 H6A 109.7 . . ? C5 C6 H6B 109.7 . . ? C7 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? N2 C7 C6 112.2(3) . . ? N2 C7 H7A 109.2 . . ? C6 C7 H7A 109.2 . . ? N2 C7 H7B 109.2 . . ? C6 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? O1 C8 N2 124.1(3) . . ? O1 C8 C9 118.2(3) . . ? N2 C8 C9 117.8(3) . . ? C10 C9 C10 120.8(3) 2_445 . ? C10 C9 C8 121.0(3) 2_445 . ? C10 C9 C8 118.0(3) . . ? C9 C10 C9 119.2(3) 3_545 . ? C9 C10 H10 120.4 3_545 . ? C9 C10 H10 120.4 . . ? O2 C11 H11A 109.5 . . ? O2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N3 C12 C13 122.2(5) . . ? N3 C12 Zn2' 47.9(3) . . ? C13 C12 Zn2' 169.9(4) . . ? N3 C12 H12A 118.9 . . ? C13 C12 H12A 118.9 . . ? Zn2' C12 H12A 71.1 . . ? C14 C13 C12 118.7(5) . . ? C14 C13 H13A 120.6 . . ? C12 C13 H13A 120.6 . . ? C13 C14 C15 118.7(5) . . ? C13 C14 H14A 120.6 . . ? C15 C14 H14A 120.6 . . ? C16 C15 C14 119.7(5) . . ? C16 C15 H15A 120.2 . . ? C14 C15 H15A 120.2 . . ? N3 C16 C15 120.8(4) . . ? N3 C16 C17 118.6(4) . . ? C15 C16 C17 120.6(4) . . ? C16 C17 C18 111.3(3) . . ? C16 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? C16 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? N4 C18 C17 111.2(3) . . ? N4 C18 H18A 109.4 . . ? C17 C18 H18A 109.4 . . ? N4 C18 H18B 109.4 . . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? O3 C19 N4 123.8(3) . . ? O3 C19 C20 119.4(3) . . ? N4 C19 C20 116.7(3) . . ? C21 C20 C21 119.7(4) 2_455 . ? C21 C20 C19 121.7(3) 2_455 . ? C21 C20 C19 118.2(3) . . ? C20 C21 C20 120.2(3) 3_445 . ? C20 C21 H21 119.9 3_445 . ? C20 C21 H21 119.9 . . ? O4 C22 H22A 109.5 . . ? O4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N5 C23 C24 120.5(3) . . ? N5 C23 C28 118.7(3) . . ? C24 C23 C28 120.8(3) . . ? C23 C24 C25 119.5(4) . . ? C23 C24 H24A 120.3 . . ? C25 C24 H24A 120.3 . . ? C26 C25 C24 118.9(4) . . ? C26 C25 H25A 120.6 . . ? C24 C25 H25A 120.6 . . ? C27 C26 C25 119.3(4) . . ? C27 C26 H26A 120.4 . . ? C25 C26 H26A 120.4 . . ? N5 C27 C26 123.5(4) . . ? N5 C27 H27A 118.3 . . ? C26 C27 H27A 118.3 . . ? C23 C28 C29 111.9(3) . . ? C23 C28 H28A 109.2 . . ? C29 C28 H28A 109.2 . . ? C23 C28 H28B 109.2 . . ? C29 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? N6 C29 C28 112.1(3) . . ? N6 C29 H29A 109.2 . . ? C28 C29 H29A 109.2 . . ? N6 C29 H29B 109.2 . . ? C28 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? O5 C30 N6 124.1(3) . . ? O5 C30 C31 119.2(3) . . ? N6 C30 C31 116.8(3) . . ? C32 C31 C32 120.7(3) . 3 ? C32 C31 C30 121.4(3) . . ? C32 C31 C30 117.6(3) 3 . ? C31 C32 C31 119.3(3) . 2 ? C31 C32 H32 120.4 . . ? C31 C32 H32 120.4 2 . ? O6 C33 H33A 109.5 . . ? O6 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O6 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.115 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.071 # 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 -0.012 0.349 1.005 57 19 ' ' 2 0.012 0.651 0.505 57 19 ' ' 3 0.349 0.361 0.505 57 19 ' ' 4 0.361 0.012 1.005 57 19 ' ' 5 0.639 0.988 0.505 57 19 ' ' 6 0.651 0.639 0.005 57 19 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 970293' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Zn3Br6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H42 Br6 N6 O6 Zn3' _chemical_formula_weight 1294.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 31.5420(3) _cell_length_b 31.5420(3) _cell_length_c 7.68620(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6622.48(12) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9874 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 22.86 _exptl_crystal_description BLOCK _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.947 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3780 _exptl_absorpt_coefficient_mu 7.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1546 _exptl_absorpt_correction_T_max 0.3174 _exptl_absorpt_process_details sadabs _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 'Bruker Breeze CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 122461 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_unetI/netI 0.0393 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 0.75 _diffrn_reflns_theta_max 28.36 _reflns_number_total 10991 _reflns_number_gt 9422 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0228P)^2^+21.5190P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.021(10) _refine_ls_number_reflns 10991 _refine_ls_number_parameters 487 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0890 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _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 -0.55589(3) -0.48607(3) -0.77128(10) 0.03836(18) Uani 1 1 d . . . Zn2 Zn -0.40844(2) -0.23096(2) -1.24612(9) 0.02524(14) Uani 1 1 d . . . Zn3 Zn -0.17818(2) -0.25661(2) -1.03996(9) 0.02463(13) Uani 1 1 d . . . Br1 Br -0.57864(2) -0.45810(3) -1.02096(10) 0.04630(17) Uani 1 1 d . . . Br2 Br -0.55842(4) -0.56099(3) -0.73787(13) 0.0661(2) Uani 1 1 d . . . Br3 Br -0.34342(2) -0.24438(2) -1.30862(9) 0.03574(14) Uani 1 1 d . . . Br4 Br -0.46531(2) -0.24311(2) -1.46975(8) 0.03266(13) Uani 1 1 d . . . Br5 Br -0.25980(2) -0.31638(2) -0.99030(9) 0.03812(15) Uani 1 1 d . . . Br6 Br -0.13324(2) -0.20232(2) -0.80960(8) 0.03084(12) Uani 1 1 d . . . O1 O -0.63099(15) -0.42272(14) -0.5786(6) 0.0302(9) Uani 1 1 d . . . O2 O -0.6101(2) -0.49385(18) -0.6064(7) 0.0527(14) Uani 1 1 d . . . H2 H -0.6242 -0.4780 -0.6313 0.063 Uiso 1 1 d R . . O3 O -0.54030(13) -0.29983(14) -1.0581(6) 0.0301(9) Uani 1 1 d . . . O4 O -0.44975(14) -0.28385(14) -1.0689(5) 0.0309(9) Uani 1 1 d . . . H4 H -0.4778 -0.2894 -1.0971 0.037 Uiso 1 1 d R . . O5 O -0.10043(13) -0.12227(12) -1.2274(6) 0.0247(8) Uani 1 1 d . . . O6 O -0.17882(14) -0.21010(14) -1.2223(6) 0.0349(10) Uani 1 1 d . . . H6 H -0.1538 -0.1828 -1.2404 0.042 Uiso 1 1 d R . . N1 N -0.48800(19) -0.43112(19) -0.6973(7) 0.0334(12) Uani 1 1 d . . . N2 N -0.57076(18) -0.36724(19) -0.4028(7) 0.0312(11) Uani 1 1 d . . . H2B H -0.5631 -0.3438 -0.3262 0.037 Uiso 1 1 calc R . . N3 N -0.38335(17) -0.16548(17) -1.1214(6) 0.0261(10) Uani 1 1 d . . . N4 N -0.53793(16) -0.24121(17) -0.8825(7) 0.0267(10) Uani 1 1 d . . . H4B H -0.5555 -0.2327 -0.8176 0.032 Uiso 1 1 calc R . . N5 N -0.14003(17) -0.28494(16) -1.1630(6) 0.0245(10) Uani 1 1 d . . . N6 N -0.04789(16) -0.13177(16) -1.4034(6) 0.0229(10) Uani 1 1 d . . . H6C H -0.0218 -0.1168 -1.4699 0.027 Uiso 1 1 calc R . . C1 C -0.4502(3) -0.4401(3) -0.7177(10) 0.049(2) Uani 1 1 d . . . H1A H -0.4574 -0.4718 -0.7539 0.059 Uiso 1 1 calc R . . C2 C -0.4019(3) -0.4051(3) -0.6883(10) 0.055(2) Uani 1 1 d . . . H2A H -0.3765 -0.4124 -0.7092 0.066 Uiso 1 1 calc R . . C3 C -0.3911(3) -0.3600(3) -0.6288(10) 0.0454(17) Uani 1 1 d . . . H3A H -0.3583 -0.3357 -0.6043 0.054 Uiso 1 1 calc R . . C4 C -0.4291(2) -0.3506(2) -0.6049(9) 0.0357(14) Uani 1 1 d . . . H4A H -0.4225 -0.3197 -0.5616 0.043 Uiso 1 1 calc R . . C5 C -0.4763(2) -0.3858(2) -0.6437(8) 0.0324(14) Uani 1 1 d . . . C6 C -0.5172(2) -0.3749(2) -0.6206(8) 0.0302(13) Uani 1 1 d . . . H6A H -0.5442 -0.3955 -0.7011 0.036 Uiso 1 1 calc R . . H6B H -0.5053 -0.3401 -0.6498 0.036 Uiso 1 1 calc R . . C7 C -0.5361(2) -0.3848(2) -0.4328(8) 0.0318(14) Uani 1 1 d . . . H7A H -0.5526 -0.4204 -0.4095 0.038 Uiso 1 1 calc R . . H7B H -0.5082 -0.3682 -0.3515 0.038 Uiso 1 1 calc R . . C8 C -0.61344(18) -0.38536(19) -0.4870(8) 0.0224(11) Uani 1 1 d . . . C9 C -0.64056(19) -0.3582(2) -0.4679(8) 0.0241(11) Uani 1 1 d . . . C10 C -0.69121(19) -0.38459(19) -0.4697(8) 0.0235(11) Uani 1 1 d . . . H10A H -0.7080 -0.4194 -0.4722 0.028 Uiso 1 1 calc R . . C11 C -0.6404(3) -0.5326(3) -0.4925(11) 0.0530(19) Uani 1 1 d . . . H11A H -0.6634 -0.5250 -0.4341 0.064 Uiso 1 1 calc R . . H11B H -0.6200 -0.5367 -0.4054 0.064 Uiso 1 1 calc R . . H11C H -0.6587 -0.5630 -0.5592 0.064 Uiso 1 1 calc R . . C12 C -0.3343(2) -0.1364(2) -1.1106(8) 0.0310(13) Uani 1 1 d . . . H12A H -0.3139 -0.1476 -1.1593 0.037 Uiso 1 1 calc R . . C13 C -0.3125(2) -0.0912(2) -1.0320(9) 0.0369(15) Uani 1 1 d . . . H13A H -0.2779 -0.0718 -1.0270 0.044 Uiso 1 1 calc R . . C14 C -0.3411(2) -0.0743(2) -0.9610(9) 0.0356(14) Uani 1 1 d . . . H14A H -0.3268 -0.0433 -0.9055 0.043 Uiso 1 1 calc R . . C15 C -0.3915(2) -0.1038(2) -0.9723(9) 0.0329(13) Uani 1 1 d . . . H15A H -0.4121 -0.0929 -0.9242 0.040 Uiso 1 1 calc R . . C16 C -0.4119(2) -0.1485(2) -1.0522(8) 0.0281(12) Uani 1 1 d . . . C17 C -0.46671(19) -0.18194(19) -1.0562(8) 0.0256(12) Uani 1 1 d . . . H17A H -0.4755 -0.2058 -1.1523 0.031 Uiso 1 1 calc R . . H17B H -0.4828 -0.1624 -1.0780 0.031 Uiso 1 1 calc R . . C18 C -0.48474(19) -0.2091(2) -0.8853(8) 0.0239(11) Uani 1 1 d . . . H18A H -0.4688 -0.2289 -0.8650 0.029 Uiso 1 1 calc R . . H18B H -0.4751 -0.1850 -0.7895 0.029 Uiso 1 1 calc R . . C19 C -0.56089(18) -0.28222(18) -0.9724(8) 0.0236(11) Uani 1 1 d . . . C20 C -0.61558(18) -0.30760(18) -0.9669(8) 0.0213(10) Uani 1 1 d . . . C21 C -0.64149(19) -0.35903(18) -0.9663(7) 0.0217(10) Uani 1 1 d . . . H21A H -0.6241 -0.3764 -0.9654 0.026 Uiso 1 1 calc R . . C22 C -0.4492(2) -0.3295(2) -1.0574(9) 0.0367(15) Uani 1 1 d . . . H22A H -0.4712 -0.3497 -0.9641 0.044 Uiso 1 1 calc R . . H22B H -0.4158 -0.3225 -1.0322 0.044 Uiso 1 1 calc R . . H22C H -0.4601 -0.3471 -1.1682 0.044 Uiso 1 1 calc R . . C23 C -0.1632(2) -0.3347(2) -1.1818(8) 0.0290(13) Uani 1 1 d . . . H23A H -0.1956 -0.3536 -1.1382 0.035 Uiso 1 1 calc R . . C24 C -0.1425(2) -0.3584(2) -1.2592(8) 0.0355(14) Uani 1 1 d . . . H24A H -0.1600 -0.3931 -1.2693 0.043 Uiso 1 1 calc R . . C25 C -0.0956(2) -0.3316(2) -1.3231(9) 0.0337(13) Uani 1 1 d . . . H25A H -0.0805 -0.3473 -1.3807 0.040 Uiso 1 1 calc R . . C26 C -0.0709(2) -0.2815(2) -1.3021(9) 0.0321(13) Uani 1 1 d . . . H26A H -0.0380 -0.2625 -1.3408 0.038 Uiso 1 1 calc R . . C27 C -0.0939(2) -0.25867(19) -1.2245(7) 0.0240(11) Uani 1 1 d . . . C28 C -0.0692(2) -0.2042(2) -1.2191(8) 0.0253(12) Uani 1 1 d . . . H28A H -0.0342 -0.1904 -1.1888 0.030 Uiso 1 1 calc R . . H28B H -0.0845 -0.1939 -1.1288 0.030 Uiso 1 1 calc R . . C29 C -0.0734(2) -0.18486(19) -1.3955(8) 0.0250(12) Uani 1 1 d . . . H29A H -0.0600 -0.1972 -1.4858 0.030 Uiso 1 1 calc R . . H29B H -0.1085 -0.1977 -1.4222 0.030 Uiso 1 1 calc R . . C30 C -0.06188(17) -0.10480(17) -1.3158(7) 0.0193(10) Uani 1 1 d . . . C31 C -0.02957(18) -0.05077(17) -1.3237(7) 0.0177(10) Uani 1 1 d . . . C32 C 0.02132(18) -0.02931(17) -1.3222(7) 0.0185(10) Uani 1 1 d . . . H32A H 0.0358 -0.0494 -1.3201 0.022 Uiso 1 1 calc R . . C33 C -0.2203(2) -0.2092(2) -1.2910(9) 0.0319(13) Uani 1 1 d . . . H33A H -0.2095 -0.1827 -1.3765 0.038 Uiso 1 1 calc R . . H33B H -0.2378 -0.2036 -1.1964 0.038 Uiso 1 1 calc R . . H33C H -0.2422 -0.2406 -1.3474 0.038 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 0.0443(4) 0.0393(4) 0.0393(5) -0.0106(3) -0.0090(3) 0.0268(3) Zn2 0.0182(3) 0.0292(3) 0.0265(3) 0.0002(3) -0.0001(3) 0.0105(3) Zn3 0.0226(3) 0.0215(3) 0.0264(3) 0.0013(3) -0.0014(3) 0.0085(3) Br1 0.0380(3) 0.0557(4) 0.0394(4) -0.0011(3) -0.0109(3) 0.0191(3) Br2 0.1008(7) 0.0520(5) 0.0685(6) -0.0134(4) -0.0084(5) 0.0555(5) Br3 0.0241(3) 0.0535(4) 0.0341(3) -0.0004(3) 0.0013(3) 0.0228(3) Br4 0.0270(3) 0.0441(3) 0.0269(3) -0.0042(3) -0.0058(2) 0.0178(3) Br5 0.0270(3) 0.0340(3) 0.0376(4) 0.0051(3) 0.0035(3) 0.0034(2) Br6 0.0324(3) 0.0311(3) 0.0274(3) -0.0055(3) -0.0031(3) 0.0147(2) O1 0.030(2) 0.024(2) 0.040(2) -0.0096(17) -0.0099(18) 0.0156(17) O2 0.067(3) 0.037(3) 0.069(4) 0.014(2) 0.027(3) 0.037(3) O3 0.0226(19) 0.028(2) 0.041(3) -0.0077(19) 0.0040(18) 0.0137(17) O4 0.0208(19) 0.034(2) 0.035(2) 0.0069(19) 0.0078(17) 0.0117(18) O5 0.0212(18) 0.0137(16) 0.034(2) 0.0020(16) 0.0099(17) 0.0052(14) O6 0.0186(19) 0.028(2) 0.050(3) 0.018(2) 0.0003(19) 0.0055(16) N1 0.038(3) 0.039(3) 0.033(3) -0.009(2) -0.005(2) 0.027(3) N2 0.030(3) 0.042(3) 0.031(3) -0.017(2) -0.012(2) 0.025(2) N3 0.019(2) 0.028(3) 0.024(2) 0.003(2) 0.0000(19) 0.006(2) N4 0.017(2) 0.030(3) 0.030(3) -0.009(2) 0.0023(19) 0.009(2) N5 0.026(2) 0.018(2) 0.026(3) -0.0009(18) -0.0052(19) 0.009(2) N6 0.024(2) 0.017(2) 0.026(2) 0.0027(18) 0.0079(19) 0.0088(19) C1 0.058(5) 0.080(6) 0.036(4) -0.012(4) -0.012(3) 0.055(5) C2 0.040(4) 0.098(7) 0.050(5) -0.024(4) -0.009(3) 0.051(5) C3 0.033(4) 0.055(5) 0.043(4) -0.006(3) -0.005(3) 0.018(3) C4 0.033(3) 0.037(4) 0.040(4) 0.002(3) -0.003(3) 0.020(3) C5 0.036(3) 0.042(4) 0.028(3) -0.002(3) -0.004(3) 0.026(3) C6 0.030(3) 0.029(3) 0.038(3) -0.005(3) -0.007(3) 0.019(3) C7 0.032(3) 0.043(4) 0.032(3) -0.006(3) -0.008(3) 0.027(3) C8 0.020(2) 0.024(3) 0.026(3) -0.005(2) -0.003(2) 0.013(2) C9 0.024(3) 0.029(3) 0.027(3) -0.001(2) -0.001(2) 0.018(2) C10 0.021(2) 0.020(2) 0.024(3) 0.000(2) -0.001(2) 0.006(2) C11 0.072(5) 0.041(4) 0.052(5) 0.015(4) 0.010(4) 0.033(4) C12 0.024(3) 0.033(3) 0.027(3) 0.006(3) 0.003(2) 0.007(3) C13 0.025(3) 0.034(3) 0.029(3) 0.003(3) -0.007(3) -0.002(3) C14 0.036(3) 0.027(3) 0.031(3) 0.004(3) -0.001(3) 0.006(3) C15 0.037(3) 0.029(3) 0.031(3) 0.001(3) -0.001(3) 0.015(3) C16 0.025(3) 0.034(3) 0.024(3) 0.006(2) -0.001(2) 0.014(2) C17 0.019(2) 0.022(3) 0.031(3) -0.001(2) -0.001(2) 0.006(2) C18 0.021(3) 0.026(3) 0.026(3) -0.004(2) -0.003(2) 0.013(2) C19 0.021(2) 0.017(2) 0.029(3) 0.002(2) 0.002(2) 0.007(2) C20 0.018(2) 0.020(2) 0.024(3) -0.001(2) -0.001(2) 0.008(2) C21 0.025(3) 0.023(3) 0.022(3) -0.002(2) -0.002(2) 0.015(2) C22 0.030(3) 0.031(3) 0.043(4) 0.004(3) -0.008(3) 0.011(3) C23 0.031(3) 0.018(3) 0.030(3) 0.000(2) -0.008(2) 0.006(2) C24 0.059(4) 0.016(3) 0.027(3) 0.000(2) -0.012(3) 0.016(3) C25 0.049(4) 0.028(3) 0.033(3) -0.002(3) 0.001(3) 0.026(3) C26 0.041(3) 0.032(3) 0.032(3) 0.006(3) 0.009(3) 0.025(3) C27 0.033(3) 0.023(3) 0.017(3) 0.000(2) 0.001(2) 0.015(2) C28 0.022(3) 0.027(3) 0.027(3) 0.000(2) 0.001(2) 0.013(2) C29 0.026(3) 0.021(3) 0.029(3) -0.001(2) 0.005(2) 0.012(2) C30 0.015(2) 0.017(2) 0.023(2) 0.002(2) -0.002(2) 0.0061(19) C31 0.021(2) 0.014(2) 0.017(2) 0.003(2) 0.002(2) 0.0074(19) C32 0.021(2) 0.019(2) 0.020(2) 0.004(2) 0.001(2) 0.013(2) C33 0.028(3) 0.027(3) 0.045(4) -0.002(3) -0.010(3) 0.016(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 O2 2.043(5) . ? Zn1 N1 2.050(5) . ? Zn1 Br2 2.3382(10) . ? Zn1 Br1 2.3686(11) . ? Zn2 O4 2.040(4) . ? Zn2 N3 2.044(5) . ? Zn2 Br3 2.3419(8) . ? Zn2 Br4 2.3729(9) . ? Zn3 O6 2.036(4) . ? Zn3 N5 2.053(5) . ? Zn3 Br5 2.3398(8) . ? Zn3 Br6 2.3769(9) . ? O1 C8 1.241(6) . ? O2 C11 1.416(8) . ? O2 H2 0.8400 . ? O3 C19 1.235(7) . ? O4 C22 1.453(7) . ? O4 H4 0.8400 . ? O5 C30 1.254(6) . ? O6 C33 1.425(6) . ? O6 H6 0.8400 . ? N1 C5 1.348(8) . ? N1 C1 1.366(8) . ? N2 C8 1.337(7) . ? N2 C7 1.470(7) . ? N2 H2B 0.8800 . ? N3 C12 1.351(7) . ? N3 C16 1.363(8) . ? N4 C19 1.318(7) . ? N4 C18 1.464(7) . ? N4 H4B 0.8800 . ? N5 C27 1.350(7) . ? N5 C23 1.368(7) . ? N6 C30 1.322(7) . ? N6 C29 1.452(7) . ? N6 H6C 0.8800 . ? C1 C2 1.380(11) . ? C1 H1A 0.9500 . ? C2 C3 1.366(11) . ? C2 H2A 0.9500 . ? C3 C4 1.381(9) . ? C3 H3A 0.9500 . ? C4 C5 1.374(9) . ? C4 H4A 0.9500 . ? C5 C6 1.503(8) . ? C6 C7 1.533(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.490(7) . ? C9 C10 1.384(7) . ? C9 C10 1.409(7) 2_455 ? C10 C9 1.409(7) 3_445 ? C10 H10A 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.375(9) . ? C12 H12A 0.9500 . ? C13 C14 1.369(9) . ? C13 H13A 0.9500 . ? C14 C15 1.387(8) . ? C14 H14A 0.9500 . ? C15 C16 1.369(8) . ? C15 H15A 0.9500 . ? C16 C17 1.510(7) . ? C17 C18 1.514(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.496(7) . ? C20 C21 1.381(7) 2_455 ? C20 C21 1.405(7) . ? C21 C20 1.381(7) 3_445 ? C21 H21A 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.353(9) . ? C23 H23A 0.9500 . ? C24 C25 1.376(9) . ? C24 H24A 0.9500 . ? C25 C26 1.378(8) . ? C25 H25A 0.9500 . ? C26 C27 1.386(8) . ? C26 H26A 0.9500 . ? C27 C28 1.491(7) . ? C28 C29 1.520(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.487(6) . ? C31 C32 1.386(7) 3 ? C31 C32 1.396(7) . ? C32 C31 1.386(7) 2 ? C32 H32A 0.9500 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 N1 112.8(2) . . ? O2 Zn1 Br2 101.95(14) . . ? N1 Zn1 Br2 108.51(15) . . ? O2 Zn1 Br1 98.95(16) . . ? N1 Zn1 Br1 107.03(15) . . ? Br2 Zn1 Br1 127.00(5) . . ? O4 Zn2 N3 106.23(18) . . ? O4 Zn2 Br3 104.38(12) . . ? N3 Zn2 Br3 110.32(13) . . ? O4 Zn2 Br4 103.27(12) . . ? N3 Zn2 Br4 112.48(14) . . ? Br3 Zn2 Br4 118.80(4) . . ? O6 Zn3 N5 102.46(19) . . ? O6 Zn3 Br5 106.83(11) . . ? N5 Zn3 Br5 111.88(13) . . ? O6 Zn3 Br6 102.16(13) . . ? N5 Zn3 Br6 112.86(13) . . ? Br5 Zn3 Br6 118.59(4) . . ? C11 O2 Zn1 130.5(4) . . ? C11 O2 H2 109.0 . . ? Zn1 O2 H2 116.6 . . ? C22 O4 Zn2 122.1(4) . . ? C22 O4 H4 110.1 . . ? Zn2 O4 H4 100.0 . . ? C33 O6 Zn3 127.6(4) . . ? C33 O6 H6 108.7 . . ? Zn3 O6 H6 120.7 . . ? C5 N1 C1 116.7(6) . . ? C5 N1 Zn1 126.7(4) . . ? C1 N1 Zn1 116.4(5) . . ? C8 N2 C7 122.8(5) . . ? C8 N2 H2B 118.6 . . ? C7 N2 H2B 118.6 . . ? C12 N3 C16 117.8(5) . . ? C12 N3 Zn2 116.6(4) . . ? C16 N3 Zn2 125.5(4) . . ? C19 N4 C18 123.3(5) . . ? C19 N4 H4B 118.3 . . ? C18 N4 H4B 118.3 . . ? C27 N5 C23 117.4(5) . . ? C27 N5 Zn3 125.5(4) . . ? C23 N5 Zn3 117.1(4) . . ? C30 N6 C29 123.3(4) . . ? C30 N6 H6C 118.3 . . ? C29 N6 H6C 118.3 . . ? N1 C1 C2 123.0(7) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C3 C2 C1 119.2(6) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C4 118.5(7) . . ? C2 C3 H3A 120.7 . . ? C4 C3 H3A 120.7 . . ? C5 C4 C3 120.1(6) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? N1 C5 C4 122.4(6) . . ? N1 C5 C6 117.8(5) . . ? C4 C5 C6 119.7(6) . . ? C5 C6 C7 110.9(5) . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N2 C7 C6 111.0(5) . . ? N2 C7 H7A 109.4 . . ? C6 C7 H7A 109.4 . . ? N2 C7 H7B 109.4 . . ? C6 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? O1 C8 N2 123.8(5) . . ? O1 C8 C9 119.3(5) . . ? N2 C8 C9 116.8(5) . . ? C10 C9 C10 120.6(5) . 2_455 ? C10 C9 C8 118.4(5) . . ? C10 C9 C8 120.6(5) 2_455 . ? C9 C10 C9 119.4(5) . 3_445 ? C9 C10 H10A 120.3 . . ? C9 C10 H10A 120.3 3_445 . ? O2 C11 H11A 109.5 . . ? O2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N3 C12 C13 122.6(6) . . ? N3 C12 H12A 118.7 . . ? C13 C12 H12A 118.7 . . ? C14 C13 C12 119.7(6) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C13 C14 C15 118.1(6) . . ? C13 C14 H14A 120.9 . . ? C15 C14 H14A 120.9 . . ? C16 C15 C14 120.6(6) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? N3 C16 C15 121.2(5) . . ? N3 C16 C17 118.0(5) . . ? C15 C16 C17 120.7(5) . . ? C16 C17 C18 110.6(5) . . ? C16 C17 H17A 109.5 . . ? C18 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? N4 C18 C17 112.4(5) . . ? N4 C18 H18A 109.1 . . ? C17 C18 H18A 109.1 . . ? N4 C18 H18B 109.1 . . ? C17 C18 H18B 109.1 . . ? H18A C18 H18B 107.9 . . ? O3 C19 N4 124.5(5) . . ? O3 C19 C20 119.9(5) . . ? N4 C19 C20 115.5(5) . . ? C21 C20 C21 119.6(5) 2_455 . ? C21 C20 C19 122.5(4) 2_455 . ? C21 C20 C19 117.9(5) . . ? C20 C21 C20 120.4(5) 3_445 . ? C20 C21 H21A 119.8 3_445 . ? C20 C21 H21A 119.8 . . ? O4 C22 H22A 109.5 . . ? O4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 N5 123.5(6) . . ? C24 C23 H23A 118.2 . . ? N5 C23 H23A 118.2 . . ? C23 C24 C25 119.0(5) . . ? C23 C24 H24A 120.5 . . ? C25 C24 H24A 120.5 . . ? C24 C25 C26 118.8(6) . . ? C24 C25 H25A 120.6 . . ? C26 C25 H25A 120.6 . . ? C25 C26 C27 120.2(6) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? N5 C27 C26 121.1(5) . . ? N5 C27 C28 118.7(5) . . ? C26 C27 C28 120.1(5) . . ? C27 C28 C29 109.7(5) . . ? C27 C28 H28A 109.7 . . ? C29 C28 H28A 109.7 . . ? C27 C28 H28B 109.7 . . ? C29 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? N6 C29 C28 113.0(5) . . ? N6 C29 H29A 109.0 . . ? C28 C29 H29A 109.0 . . ? N6 C29 H29B 109.0 . . ? C28 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? O5 C30 N6 123.7(4) . . ? O5 C30 C31 119.0(5) . . ? N6 C30 C31 117.3(4) . . ? C32 C31 C32 119.7(5) 3 . ? C32 C31 C30 119.0(4) 3 . ? C32 C31 C30 121.2(4) . . ? C31 C32 C31 120.3(5) 2 . ? C31 C32 H32A 119.8 2 . ? C31 C32 H32A 119.8 . . ? O6 C33 H33A 109.5 . . ? O6 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O6 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.842 _refine_diff_density_min -0.995 _refine_diff_density_rms 0.114 _database_code_depnum_ccdc_archive 'CCDC 970294' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Zn3I6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H42 I6 N6 O6 Zn3' _chemical_formula_weight 1576.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 31.9496(2) _cell_length_b 31.9496(2) _cell_length_c 8.02110(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7090.80(11) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9840 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 27.73 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4428 _exptl_absorpt_coefficient_mu 5.473 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2019 _exptl_absorpt_correction_T_max 0.2302 _exptl_absorpt_process_details sadabs _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 'Bruker Breeze CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39189 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_unetI/netI 0.0551 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 0.74 _diffrn_reflns_theta_max 28.26 _reflns_number_total 11188 _reflns_number_gt 9796 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0223P)^2^+30.5919P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(2) _refine_ls_number_reflns 11188 _refine_ls_number_parameters 487 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0895 _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_restrained_S_all 1.188 _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 0.77189(3) 0.59281(3) 1.11954(14) 0.0227(2) Uani 1 1 d . . . Zn2 Zn 0.55584(4) 0.07074(4) 0.64245(15) 0.0308(3) Uani 1 1 d . . . Zn3 Zn 0.82565(3) 0.08506(3) 0.41322(13) 0.0220(2) Uani 1 1 d . . . I1 I 0.76193(2) 0.53641(2) 1.36336(8) 0.02825(13) Uani 1 1 d . . . I2 I 0.75588(2) 0.66106(2) 1.18350(8) 0.03341(15) Uani 1 1 d . . . I3 I 0.57704(2) 0.12217(2) 0.90965(8) 0.03640(16) Uani 1 1 d . . . I4 I 0.56216(3) -0.00454(3) 0.61306(11) 0.0507(2) Uani 1 1 d . . . I5 I 0.73820(2) 0.06199(2) 0.36670(9) 0.03431(15) Uani 1 1 d . . . I6 I 0.87109(2) 0.07618(2) 0.16246(8) 0.02657(13) Uani 1 1 d . . . O1 O 0.7018(2) 0.4589(2) 0.9441(10) 0.0371(18) Uani 1 1 d . . . O2 O 0.7201(2) 0.5487(2) 0.9513(8) 0.0271(15) Uani 1 1 d . . . H2C H 0.7151 0.5240 1.0300 0.033 Uiso 1 1 d R . . O3 O 0.6289(2) 0.2090(2) 0.4707(9) 0.0317(16) Uani 1 1 d . . . O4 O 0.6074(3) 0.1173(3) 0.4822(10) 0.046(2) Uani 1 1 d . . . H4C H 0.6201 0.1513 0.4984 0.055 Uiso 1 1 d R . . O5 O 0.9029(2) 0.0260(2) 0.5729(9) 0.0293(16) Uani 1 1 d . . . O6 O 0.8269(2) 0.0377(2) 0.5784(9) 0.0342(17) Uani 1 1 d . . . H6D H 0.8456 0.0273 0.5155 0.041 Uiso 1 1 d R . . N1 N 0.8350(2) 0.6153(3) 0.9918(9) 0.0220(16) Uani 1 1 d . . . N2 N 0.7608(3) 0.4596(2) 0.7812(9) 0.0222(16) Uani 1 1 d . . . H2B H 0.7698 0.4419 0.7242 0.027 Uiso 1 1 calc R . . N3 N 0.4884(3) 0.0584(2) 0.5750(9) 0.0255(18) Uani 1 1 d . . . N4 N 0.5703(3) 0.2066(2) 0.3073(10) 0.0298(19) Uani 1 1 d . . . H4B H 0.5632 0.2234 0.2380 0.036 Uiso 1 1 calc R . . N5 N 0.8637(3) 0.1480(3) 0.5434(9) 0.0236(17) Uani 1 1 d . . . N6 N 0.9574(2) 0.0864(2) 0.7403(10) 0.0225(17) Uani 1 1 d . . . H6C H 0.9842 0.0971 0.7981 0.027 Uiso 1 1 calc R . . C1 C 0.8645(3) 0.6633(3) 0.9751(11) 0.030(2) Uani 1 1 d . . . H1A H 0.8543 0.6843 1.0201 0.036 Uiso 1 1 calc R . . C2 C 0.9077(3) 0.6831(3) 0.8977(13) 0.035(2) Uani 1 1 d . . . H2A H 0.9267 0.7172 0.8846 0.042 Uiso 1 1 calc R . . C3 C 0.9243(4) 0.6531(4) 0.8371(13) 0.041(3) Uani 1 1 d . . . H3A H 0.9549 0.6663 0.7846 0.049 Uiso 1 1 calc R . . C4 C 0.8952(3) 0.6038(3) 0.8551(14) 0.034(2) Uani 1 1 d . . . H4A H 0.9056 0.5824 0.8164 0.041 Uiso 1 1 calc R . . C5 C 0.8511(3) 0.5863(3) 0.9298(11) 0.0216(19) Uani 1 1 d . . . C6 C 0.8174(3) 0.5326(3) 0.9436(11) 0.0212(19) Uani 1 1 d . . . H6A H 0.7929 0.5260 1.0309 0.025 Uiso 1 1 calc R . . H6B H 0.8359 0.5168 0.9769 0.025 Uiso 1 1 calc R . . C7 C 0.7922(3) 0.5119(3) 0.7787(12) 0.0224(19) Uani 1 1 d . . . H7A H 0.7726 0.5270 0.7488 0.027 Uiso 1 1 calc R . . H7B H 0.8169 0.5205 0.6909 0.027 Uiso 1 1 calc R . . C8 C 0.7194(3) 0.4372(3) 0.8647(13) 0.0244(19) Uani 1 1 d . . . C9 C 0.6929(3) 0.3839(3) 0.8624(12) 0.0212(18) Uani 1 1 d . . . C10 C 0.6426(3) 0.3595(3) 0.8632(12) 0.0221(18) Uani 1 1 d . . . H10A H 0.6261 0.3773 0.8643 0.027 Uiso 1 1 calc R . . C11 C 0.6767(3) 0.5498(3) 0.9325(14) 0.034(2) Uani 1 1 d . . . H11A H 0.6568 0.5268 0.8460 0.041 Uiso 1 1 calc R . . H11B H 0.6842 0.5825 0.9002 0.041 Uiso 1 1 calc R . . H11C H 0.6590 0.5411 1.0384 0.041 Uiso 1 1 calc R . . C12 C 0.4519(4) 0.0128(4) 0.5926(14) 0.043(3) Uani 1 1 d . . . H12A H 0.4599 -0.0112 0.6221 0.052 Uiso 1 1 calc R . . C13 C 0.4034(4) -0.0020(4) 0.5709(14) 0.046(3) Uani 1 1 d . . . H13A H 0.3789 -0.0345 0.5908 0.055 Uiso 1 1 calc R . . C14 C 0.3923(4) 0.0324(4) 0.5192(14) 0.044(3) Uani 1 1 d . . . H14A H 0.3597 0.0239 0.4982 0.052 Uiso 1 1 calc R . . C15 C 0.4297(3) 0.0800(3) 0.4983(12) 0.029(2) Uani 1 1 d . . . H15A H 0.4228 0.1043 0.4640 0.035 Uiso 1 1 calc R . . C16 C 0.4767(3) 0.0914(3) 0.5277(11) 0.0228(19) Uani 1 1 d . . . C17 C 0.5162(3) 0.1430(3) 0.5072(12) 0.025(2) Uani 1 1 d . . . H17A H 0.5433 0.1494 0.5826 0.030 Uiso 1 1 calc R . . H17B H 0.5038 0.1647 0.5401 0.030 Uiso 1 1 calc R . . C18 C 0.5347(3) 0.1544(3) 0.3294(12) 0.029(2) Uani 1 1 d . . . H18A H 0.5502 0.1351 0.3001 0.035 Uiso 1 1 calc R . . H18B H 0.5072 0.1450 0.2526 0.035 Uiso 1 1 calc R . . C19 C 0.6119(3) 0.2288(3) 0.3865(12) 0.0229(19) Uani 1 1 d . . . C20 C 0.6401(3) 0.2834(3) 0.3701(12) 0.0206(18) Uani 1 1 d . . . C21 C 0.6163(3) 0.3100(3) 0.3703(12) 0.0233(19) Uani 1 1 d . . . H21A H 0.5820 0.2940 0.3706 0.028 Uiso 1 1 calc R . . C22 C 0.6373(4) 0.1105(4) 0.3694(15) 0.050(3) Uani 1 1 d . . . H22A H 0.6579 0.1407 0.3095 0.060 Uiso 1 1 calc R . . H22B H 0.6173 0.0851 0.2894 0.060 Uiso 1 1 calc R . . H22C H 0.6577 0.1009 0.4309 0.060 Uiso 1 1 calc R . . C23 C 0.8421(4) 0.1745(3) 0.5725(11) 0.026(2) Uani 1 1 d . . . H23A H 0.8097 0.1618 0.5365 0.031 Uiso 1 1 calc R . . C24 C 0.8643(3) 0.2188(3) 0.6512(12) 0.030(2) Uani 1 1 d . . . H24A H 0.8475 0.2360 0.6680 0.036 Uiso 1 1 calc R . . C25 C 0.9098(4) 0.2370(3) 0.7034(12) 0.030(2) Uani 1 1 d . . . H25A H 0.9255 0.2669 0.7615 0.035 Uiso 1 1 calc R . . C26 C 0.9339(3) 0.2122(3) 0.6726(12) 0.027(2) Uani 1 1 d . . . H26A H 0.9669 0.2260 0.7032 0.033 Uiso 1 1 calc R . . C27 C 0.9102(3) 0.1671(3) 0.5968(11) 0.0222(19) Uani 1 1 d . . . C28 C 0.9349(3) 0.1381(3) 0.5784(11) 0.0223(19) Uani 1 1 d . . . H28A H 0.9689 0.1594 0.5438 0.027 Uiso 1 1 calc R . . H28B H 0.9185 0.1131 0.4915 0.027 Uiso 1 1 calc R . . C29 C 0.9333(3) 0.1144(3) 0.7432(11) 0.0210(19) Uani 1 1 d . . . H29A H 0.9486 0.1397 0.8297 0.025 Uiso 1 1 calc R . . H29B H 0.8992 0.0930 0.7753 0.025 Uiso 1 1 calc R . . C30 C 0.9414(3) 0.0456(3) 0.6556(12) 0.0203(18) Uani 1 1 d . . . C31 C 0.9725(3) 0.0231(2) 0.6563(10) 0.0149(16) Uani 1 1 d . . . C32 C 1.0224(3) 0.0503(3) 0.6598(11) 0.0189(17) Uani 1 1 d . . . H32A H 1.0379 0.0845 0.6647 0.023 Uiso 1 1 calc R . . C33 C 0.7871(3) -0.0024(3) 0.6511(15) 0.040(3) Uani 1 1 d . . . H33A H 0.7986 -0.0191 0.7246 0.048 Uiso 1 1 calc R . . H33B H 0.7667 -0.0246 0.5634 0.048 Uiso 1 1 calc R . . H33C H 0.7683 0.0084 0.7161 0.048 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 0.0228(5) 0.0159(5) 0.0280(6) -0.0006(4) -0.0006(5) 0.0086(4) Zn2 0.0309(6) 0.0213(5) 0.0390(7) 0.0002(5) -0.0046(5) 0.0122(5) Zn3 0.0186(5) 0.0223(5) 0.0279(6) 0.0007(5) 0.0006(4) 0.0123(4) I1 0.0336(3) 0.0224(3) 0.0290(3) 0.0054(3) 0.0048(3) 0.0142(2) I2 0.0488(4) 0.0214(3) 0.0352(4) -0.0004(3) 0.0016(3) 0.0215(3) I3 0.0279(3) 0.0393(4) 0.0384(4) -0.0085(3) -0.0084(3) 0.0142(3) I4 0.0733(5) 0.0301(4) 0.0582(5) 0.0017(4) -0.0079(4) 0.0329(4) I5 0.0236(3) 0.0478(4) 0.0374(4) -0.0038(3) -0.0050(3) 0.0223(3) I6 0.0262(3) 0.0265(3) 0.0292(3) -0.0035(3) 0.0019(3) 0.0148(2) O1 0.028(4) 0.019(3) 0.066(5) -0.012(3) 0.005(3) 0.012(3) O2 0.017(3) 0.027(3) 0.039(4) -0.005(3) -0.010(3) 0.012(3) O3 0.025(3) 0.017(3) 0.055(5) 0.005(3) -0.003(3) 0.012(3) O4 0.046(5) 0.029(4) 0.061(5) 0.014(4) 0.026(4) 0.018(4) O5 0.023(3) 0.017(3) 0.047(4) -0.010(3) -0.013(3) 0.010(3) O6 0.028(4) 0.030(4) 0.046(4) 0.017(3) 0.006(3) 0.016(3) N1 0.017(4) 0.021(4) 0.026(4) -0.001(3) 0.003(3) 0.007(3) N2 0.026(4) 0.014(4) 0.027(4) -0.001(3) 0.003(3) 0.011(3) N3 0.026(4) 0.016(4) 0.031(4) -0.009(3) -0.009(3) 0.009(3) N4 0.026(4) 0.010(3) 0.043(5) 0.010(3) -0.004(4) 0.000(3) N5 0.032(4) 0.025(4) 0.024(4) 0.005(3) 0.006(3) 0.021(4) N6 0.017(4) 0.018(4) 0.037(4) -0.006(3) -0.009(3) 0.012(3) C1 0.031(5) 0.027(5) 0.019(5) -0.006(4) 0.001(4) 0.005(4) C2 0.037(5) 0.023(5) 0.030(6) 0.000(4) -0.008(5) 0.005(4) C3 0.028(5) 0.053(7) 0.030(6) -0.004(5) -0.001(5) 0.012(5) C4 0.021(5) 0.031(5) 0.043(6) 0.014(5) 0.005(5) 0.008(4) C5 0.014(4) 0.018(4) 0.025(5) 0.006(4) -0.002(4) 0.002(3) C6 0.030(5) 0.013(4) 0.027(5) -0.004(4) 0.003(4) 0.015(4) C7 0.017(4) 0.015(4) 0.033(5) 0.001(4) 0.007(4) 0.006(4) C8 0.024(4) 0.020(4) 0.034(5) -0.005(4) -0.002(4) 0.014(4) C9 0.023(4) 0.019(4) 0.022(4) -0.004(4) 0.002(4) 0.011(3) C10 0.025(4) 0.020(4) 0.029(5) 0.000(4) 0.002(4) 0.017(4) C11 0.025(5) 0.021(5) 0.048(6) 0.006(5) -0.015(5) 0.006(4) C12 0.053(7) 0.028(5) 0.034(6) 0.008(5) -0.013(5) 0.009(5) C13 0.030(6) 0.029(6) 0.054(8) 0.016(5) -0.011(5) -0.004(5) C14 0.044(7) 0.043(7) 0.046(7) -0.002(5) 0.000(5) 0.024(6) C15 0.032(5) 0.025(5) 0.035(6) -0.003(4) 0.000(5) 0.017(4) C16 0.027(5) 0.020(4) 0.024(5) -0.011(4) -0.011(4) 0.013(4) C17 0.024(5) 0.018(5) 0.032(5) -0.006(4) -0.007(4) 0.009(4) C18 0.018(4) 0.020(5) 0.042(6) -0.002(4) -0.011(4) 0.005(4) C19 0.015(4) 0.012(4) 0.034(6) 0.004(4) -0.002(4) 0.001(3) C20 0.011(4) 0.010(4) 0.040(5) -0.001(4) 0.003(4) 0.005(3) C21 0.022(4) 0.009(4) 0.035(5) 0.008(4) 0.001(4) 0.005(3) C22 0.066(8) 0.039(6) 0.047(7) -0.006(6) 0.019(7) 0.026(6) C23 0.037(5) 0.023(5) 0.023(5) 0.004(4) 0.007(4) 0.020(4) C24 0.055(6) 0.029(5) 0.025(5) -0.005(4) -0.006(5) 0.036(5) C25 0.044(6) 0.032(5) 0.023(5) -0.002(4) -0.005(4) 0.026(5) C26 0.034(5) 0.021(4) 0.025(5) 0.000(4) -0.010(5) 0.013(4) C27 0.018(4) 0.015(4) 0.024(5) 0.005(4) 0.004(4) 0.001(3) C28 0.025(5) 0.025(5) 0.028(5) -0.006(4) 0.001(4) 0.021(4) C29 0.014(4) 0.030(5) 0.025(5) 0.000(4) 0.001(4) 0.015(4) C30 0.021(4) 0.014(4) 0.031(5) -0.001(4) 0.002(4) 0.012(3) C31 0.019(4) 0.006(3) 0.019(4) -0.005(3) -0.006(4) 0.006(3) C32 0.017(4) 0.016(4) 0.030(5) 0.008(4) 0.006(4) 0.013(3) C33 0.035(5) 0.019(4) 0.065(8) 0.026(5) 0.025(6) 0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.044(7) . ? Zn1 O2 2.052(6) . ? Zn1 I2 2.5292(11) . ? Zn1 I1 2.5689(12) . ? Zn2 O4 2.032(7) . ? Zn2 N3 2.058(7) . ? Zn2 I4 2.5233(12) . ? Zn2 I3 2.5766(13) . ? Zn3 O6 2.026(6) . ? Zn3 N5 2.042(7) . ? Zn3 I5 2.5355(11) . ? Zn3 I6 2.5779(12) . ? O1 C8 1.263(10) . ? O2 C11 1.414(10) . ? O3 C19 1.221(10) . ? O4 C22 1.410(12) . ? O5 C30 1.255(10) . ? O6 C33 1.403(10) . ? N1 C1 1.347(11) . ? N1 C5 1.357(11) . ? N2 C8 1.328(11) . ? N2 C7 1.455(10) . ? N3 C16 1.341(11) . ? N3 C12 1.344(12) . ? N4 C19 1.317(11) . ? N4 C18 1.486(10) . ? N5 C23 1.352(11) . ? N5 C27 1.364(11) . ? N6 C30 1.327(10) . ? N6 C29 1.441(10) . ? C1 C2 1.349(13) . ? C2 C3 1.395(14) . ? C3 C4 1.378(13) . ? C4 C5 1.369(12) . ? C5 C6 1.506(11) . ? C6 C7 1.518(12) . ? C8 C9 1.474(11) . ? C9 C10 1.393(11) . ? C9 C10 1.397(11) 3_665 ? C10 C9 1.397(11) 2_655 ? C12 C13 1.388(15) . ? C13 C14 1.376(15) . ? C14 C15 1.398(14) . ? C15 C16 1.375(12) . ? C16 C17 1.501(12) . ? C17 C18 1.517(13) . ? C19 C20 1.517(10) . ? C20 C21 1.382(10) 2_655 ? C20 C21 1.397(10) . ? C21 C20 1.382(10) 3_665 ? C23 C24 1.378(12) . ? C24 C25 1.335(13) . ? C25 C26 1.375(12) . ? C26 C27 1.389(12) . ? C27 C28 1.491(11) . ? C28 C29 1.512(12) . ? C30 C31 1.486(10) . ? C31 C32 1.384(11) . ? C31 C32 1.414(10) 2_645 ? C32 C31 1.414(10) 3_765 ? 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 O2 103.1(3) . . ? N1 Zn1 I2 112.8(2) . . ? O2 Zn1 I2 106.52(17) . . ? N1 Zn1 I1 112.5(2) . . ? O2 Zn1 I1 104.15(18) . . ? I2 Zn1 I1 116.29(5) . . ? O4 Zn2 N3 111.2(3) . . ? O4 Zn2 I4 102.5(2) . . ? N3 Zn2 I4 111.54(19) . . ? O4 Zn2 I3 101.6(2) . . ? N3 Zn2 I3 104.9(2) . . ? I4 Zn2 I3 124.38(5) . . ? O6 Zn3 N5 100.2(3) . . ? O6 Zn3 I5 107.99(18) . . ? N5 Zn3 I5 112.9(2) . . ? O6 Zn3 I6 101.9(2) . . ? N5 Zn3 I6 114.6(2) . . ? I5 Zn3 I6 116.90(5) . . ? C11 O2 Zn1 121.1(6) . . ? C22 O4 Zn2 131.1(6) . . ? C33 O6 Zn3 127.4(6) . . ? C1 N1 C5 116.8(7) . . ? C1 N1 Zn1 117.1(6) . . ? C5 N1 Zn1 125.9(6) . . ? C8 N2 C7 123.7(7) . . ? C16 N3 C12 116.8(8) . . ? C16 N3 Zn2 127.0(6) . . ? C12 N3 Zn2 116.0(7) . . ? C19 N4 C18 123.1(7) . . ? C23 N5 C27 116.8(8) . . ? C23 N5 Zn3 117.8(6) . . ? C27 N5 Zn3 125.4(6) . . ? C30 N6 C29 123.8(7) . . ? N1 C1 C2 123.4(9) . . ? C1 C2 C3 119.2(9) . . ? C4 C3 C2 118.7(9) . . ? C5 C4 C3 118.7(10) . . ? N1 C5 C4 123.2(8) . . ? N1 C5 C6 116.8(7) . . ? C4 C5 C6 120.0(8) . . ? C5 C6 C7 110.8(7) . . ? N2 C7 C6 113.5(7) . . ? O1 C8 N2 123.7(7) . . ? O1 C8 C9 118.9(8) . . ? N2 C8 C9 117.4(7) . . ? C10 C9 C10 119.3(8) . 3_665 ? C10 C9 C8 118.9(7) . . ? C10 C9 C8 121.8(7) 3_665 . ? C9 C10 C9 120.7(8) . 2_655 ? N3 C12 C13 124.9(10) . . ? C14 C13 C12 117.2(10) . . ? C13 C14 C15 118.8(10) . . ? C16 C15 C14 119.8(9) . . ? N3 C16 C15 122.4(8) . . ? N3 C16 C17 118.9(8) . . ? C15 C16 C17 118.7(8) . . ? C16 C17 C18 112.3(7) . . ? N4 C18 C17 111.7(7) . . ? O3 C19 N4 125.4(7) . . ? O3 C19 C20 118.7(7) . . ? N4 C19 C20 115.9(7) . . ? C21 C20 C21 120.9(8) 2_655 . ? C21 C20 C19 118.3(7) 2_655 . ? C21 C20 C19 120.6(7) . . ? C20 C21 C20 119.1(8) 3_665 . ? N5 C23 C24 124.0(9) . . ? C25 C24 C23 118.7(8) . . ? C24 C25 C26 119.5(9) . . ? C25 C26 C27 120.5(8) . . ? N5 C27 C26 120.3(8) . . ? N5 C27 C28 119.3(7) . . ? C26 C27 C28 120.4(8) . . ? C27 C28 C29 109.2(7) . . ? N6 C29 C28 113.8(7) . . ? O5 C30 N6 124.0(7) . . ? O5 C30 C31 119.1(7) . . ? N6 C30 C31 116.8(7) . . ? C32 C31 C32 119.2(8) . 2_645 ? C32 C31 C30 122.4(6) . . ? C32 C31 C30 118.3(7) 2_645 . ? C31 C32 C31 120.7(8) . 3_765 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.991 _refine_diff_density_min -1.090 _refine_diff_density_rms 0.186 _database_code_depnum_ccdc_archive 'CCDC 970295'