data_compound2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H8 O20 Zn3, 2(C2 H8 N)' _chemical_formula_sum 'C28 H24 N2 O20 Zn3' _chemical_formula_weight 904.60 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' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7693(10) _cell_length_b 12.7842(9) _cell_length_c 14.7758(11) _cell_angle_alpha 85.019(2) _cell_angle_beta 65.8700(10) _cell_angle_gamma 89.613(2) _cell_volume 2191.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 1.698 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.7276 _exptl_absorpt_correction_T_max 0.8486 _exptl_absorpt_process_details 'multi-scan absorption correction' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42640 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0132 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.70 _reflns_number_total 11299 _reflns_number_gt 10415 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELX-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^ > 2\s(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. The structure was solved by direct methods and subsequent difference Fourier syntheses. The electron density contributionof the diffuse scattering of the disordered guest molecules was handled using SQUEEZE procedure in the PLATON software suite ; _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^)+(0.0561P)^2^+1.7639P] 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 11299 _refine_ls_number_parameters 485 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.009 _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 C1 C 0.26509(15) 0.37997(15) 0.06895(14) 0.0236(3) Uani 1 1 d . . . C2 C 0.19927(16) 0.33185(15) 0.17113(14) 0.0236(3) Uani 1 1 d . . . C3 C 0.18196(19) 0.36203(17) 0.26181(15) 0.0302(4) Uani 1 1 d . . . H3 H 0.2132 0.4215 0.2747 0.036 Uiso 1 1 calc R . . C4 C 0.10655(19) 0.28451(17) 0.33314(15) 0.0297(4) Uani 1 1 d . . . H4 H 0.0786 0.2833 0.4021 0.036 Uiso 1 1 calc R . . C5 C 0.08348(15) 0.21286(15) 0.28099(13) 0.0220(3) Uani 1 1 d . . . C6 C 0.00599(15) 0.11849(14) 0.31046(13) 0.0204(3) Uani 1 1 d . . . C7 C -0.11435(17) -0.15325(14) 0.41578(13) 0.0223(3) Uani 1 1 d . . . C8 C -0.09417(18) -0.25005(15) 0.36389(15) 0.0263(4) Uani 1 1 d . . . C9 C -0.0090(2) -0.31970(18) 0.3427(2) 0.0378(5) Uani 1 1 d . . . H9 H 0.0503 -0.3211 0.3639 0.045 Uiso 1 1 calc R . . C10 C -0.0288(2) -0.39057(19) 0.2814(2) 0.0399(5) Uani 1 1 d . . . H10 H 0.0156 -0.4472 0.2544 0.048 Uiso 1 1 calc R . . C11 C -0.12451(19) -0.35936(16) 0.27026(16) 0.0292(4) Uani 1 1 d . . . C12 C 0.18340(18) 0.39754(16) -0.21080(16) 0.0284(4) Uani 1 1 d . . . C13 C -0.23266(15) 0.07116(15) 0.63195(13) 0.0217(3) Uani 1 1 d . . . C14 C -0.26304(16) 0.12619(15) 0.72258(14) 0.0233(3) Uani 1 1 d . . . C15 C -0.22118(19) 0.12111(18) 0.79356(17) 0.0320(4) Uani 1 1 d . . . H15 H -0.1639 0.0779 0.7972 0.038 Uiso 1 1 calc R . . C16 C -0.2823(2) 0.19508(19) 0.86143(17) 0.0338(5) Uani 1 1 d . . . H16 H -0.2733 0.2098 0.9184 0.041 Uiso 1 1 calc R . . C17 C -0.35676(17) 0.23999(15) 0.82597(15) 0.0254(4) Uani 1 1 d . . . C18 C 0.55454(16) 0.31947(15) -0.13587(14) 0.0239(3) Uani 1 1 d . . . C19 C 0.45122(15) 0.60590(14) -0.17412(13) 0.0198(3) Uani 1 1 d . . . C20 C 0.47381(16) 0.70450(15) -0.23987(14) 0.0238(4) Uani 1 1 d . . . C21 C 0.56495(19) 0.77308(18) -0.2822(2) 0.0377(5) Uani 1 1 d . . . H21 H 0.6332 0.7703 -0.2736 0.045 Uiso 1 1 calc R . . C22 C 0.5350(2) 0.8501(2) -0.3422(2) 0.0415(6) Uani 1 1 d . . . H22 H 0.5804 0.9071 -0.3818 0.050 Uiso 1 1 calc R . . C23 C 0.42779(18) 0.82417(17) -0.33039(16) 0.0293(4) Uani 1 1 d . . . C24 C -0.3498(2) 0.12656(19) 0.37215(18) 0.0358(5) Uani 1 1 d . . . C25 C 0.0560(3) 0.6919(2) -0.1211(3) 0.0525(7) Uani 1 1 d . . . H31A H 0.0108 0.6285 -0.1097 0.079 Uiso 1 1 calc R . . H31B H 0.0835 0.7180 -0.1900 0.079 Uiso 1 1 calc R . . H31C H 0.0096 0.7436 -0.0804 0.079 Uiso 1 1 calc R . . C26 C 0.1231(3) 0.6288(2) 0.0089(2) 0.0475(6) Uani 1 1 d . . . H32A H 0.0874 0.6827 0.0519 0.071 Uiso 1 1 calc R . . H32B H 0.1909 0.6071 0.0174 0.071 Uiso 1 1 calc R . . H32C H 0.0705 0.5697 0.0255 0.071 Uiso 1 1 calc R . . C27 C -0.5269(5) 0.2555(4) 0.5804(4) 0.1046(18) Uani 1 1 d . . . H34A H -0.5831 0.3086 0.5905 0.157 Uiso 1 1 calc R . . H34B H -0.4803 0.2546 0.5104 0.157 Uiso 1 1 calc R . . H34C H -0.4791 0.2706 0.6140 0.157 Uiso 1 1 calc R . . C28 C -0.5953(4) 0.1200(4) 0.7193(4) 0.0853(12) Uani 1 1 d . . . H33A H -0.5233 0.1292 0.7241 0.128 Uiso 1 1 calc R . . H33B H -0.6184 0.0470 0.7331 0.128 Uiso 1 1 calc R . . H33C H -0.6525 0.1599 0.7667 0.128 Uiso 1 1 calc R . . N1 N 0.15442(15) 0.66977(14) -0.09532(15) 0.0309(4) Uani 1 1 d . . . H1A H 0.1984 0.6228 -0.1353 0.037 Uiso 1 1 calc R . . H1B H 0.1971 0.7294 -0.1078 0.037 Uiso 1 1 calc R . . N2 N -0.5829(5) 0.1566(4) 0.6189(4) 0.135(2) Uani 1 1 d . . . H2A H -0.5437 0.1087 0.5775 0.162 Uiso 1 1 calc R . . H2B H -0.6533 0.1593 0.6188 0.162 Uiso 1 1 calc R . . O1 O 0.25734(14) 0.33340(13) -0.00054(11) 0.0331(3) Uani 1 1 d . . . O2 O 0.32040(11) 0.46396(11) 0.05710(11) 0.0259(3) Uani 1 1 d . . . O3 O 0.13998(11) 0.23971(11) 0.18111(10) 0.0233(3) Uani 1 1 d . . . O4 O -0.00256(14) 0.06644(12) 0.24826(11) 0.0320(3) Uani 1 1 d . . . O5 O -0.05449(10) 0.10176(10) 0.40651(9) 0.0196(2) Uani 1 1 d . . . O6 O -0.20070(12) -0.10081(11) 0.41959(11) 0.0272(3) Uani 1 1 d . . . O7 O -0.04310(13) -0.13244(11) 0.44964(11) 0.0260(3) Uani 1 1 d . . . O8 O -0.16679(12) -0.27278(11) 0.32045(11) 0.0254(3) Uani 1 1 d . . . O9 O 0.14176(15) 0.47030(15) -0.15991(15) 0.0456(5) Uani 1 1 d . . . O10 O 0.27315(13) 0.34896(12) -0.21579(12) 0.0305(3) Uani 1 1 d . . . O11 O -0.28388(12) 0.09677(12) 0.57604(10) 0.0278(3) Uani 1 1 d . . . O12 O -0.15857(11) 0.00296(11) 0.61708(10) 0.0248(3) Uani 1 1 d . . . O13 O -0.34674(12) 0.19904(11) 0.74108(10) 0.0250(3) Uani 1 1 d . . . O14 O 0.49426(13) 0.33907(12) -0.18524(11) 0.0309(3) Uani 1 1 d . . . O15 O 0.54625(13) 0.35773(11) -0.05877(11) 0.0274(3) Uani 1 1 d . . . O16 O 0.36229(12) 0.55381(10) -0.16413(11) 0.0254(3) Uani 1 1 d . . . O17 O 0.51971(11) 0.58240(11) -0.13619(10) 0.0240(3) Uani 1 1 d . . . O18 O 0.38857(11) 0.73469(11) -0.26919(10) 0.0243(3) Uani 1 1 d . . . O19 O -0.25154(15) 0.16190(17) 0.34624(13) 0.0442(4) Uani 1 1 d . . . O20 O -0.3862(2) 0.04762(19) 0.4326(2) 0.0730(8) Uani 1 1 d . . . Zn1 Zn 0.343786(18) 0.402721(16) -0.132753(15) 0.01979(6) Uani 1 1 d . . . Zn2 Zn -0.215161(17) 0.048732(16) 0.440998(15) 0.01933(6) Uani 1 1 d . . . Zn3 Zn 0.5000 0.5000 0.0000 0.01581(6) Uani 1 2 d S . . Zn4 Zn 0.0000 0.0000 0.5000 0.01572(6) Uani 1 2 d S . . 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 C1 0.0185(8) 0.0282(9) 0.0241(9) 0.0036(7) -0.0097(7) -0.0004(6) C2 0.0209(8) 0.0263(9) 0.0240(9) 0.0022(7) -0.0105(7) -0.0036(7) C3 0.0345(10) 0.0320(10) 0.0259(9) -0.0002(8) -0.0145(8) -0.0079(8) C4 0.0345(10) 0.0340(10) 0.0206(9) -0.0006(8) -0.0115(8) -0.0059(8) C5 0.0210(8) 0.0266(9) 0.0173(8) 0.0018(6) -0.0076(6) -0.0003(7) C6 0.0192(7) 0.0236(8) 0.0188(8) 0.0001(6) -0.0084(6) 0.0018(6) C7 0.0296(9) 0.0208(8) 0.0202(8) -0.0022(6) -0.0138(7) -0.0017(7) C8 0.0350(10) 0.0232(9) 0.0303(9) -0.0059(7) -0.0223(8) -0.0009(7) C9 0.0460(13) 0.0329(11) 0.0536(14) -0.0176(10) -0.0371(12) 0.0092(9) C10 0.0459(13) 0.0326(11) 0.0579(15) -0.0239(11) -0.0346(12) 0.0124(9) C11 0.0354(10) 0.0250(9) 0.0349(10) -0.0124(8) -0.0205(9) 0.0021(8) C12 0.0307(9) 0.0288(10) 0.0303(10) -0.0101(8) -0.0156(8) -0.0026(8) C13 0.0180(7) 0.0245(8) 0.0198(8) -0.0036(6) -0.0046(6) 0.0028(6) C14 0.0204(8) 0.0258(9) 0.0237(8) -0.0074(7) -0.0083(7) 0.0088(7) C15 0.0308(10) 0.0382(11) 0.0340(11) -0.0145(9) -0.0184(9) 0.0160(8) C16 0.0362(11) 0.0405(12) 0.0344(11) -0.0185(9) -0.0215(9) 0.0153(9) C17 0.0277(9) 0.0257(9) 0.0249(9) -0.0094(7) -0.0116(7) 0.0073(7) C18 0.0253(8) 0.0207(8) 0.0244(9) -0.0056(7) -0.0082(7) 0.0050(7) C19 0.0203(8) 0.0204(8) 0.0196(8) -0.0009(6) -0.0091(6) 0.0032(6) C20 0.0220(8) 0.0265(9) 0.0272(9) 0.0027(7) -0.0153(7) 0.0020(7) C21 0.0277(10) 0.0355(11) 0.0531(14) 0.0182(10) -0.0239(10) -0.0064(8) C22 0.0341(11) 0.0382(12) 0.0529(14) 0.0216(11) -0.0234(11) -0.0062(9) C23 0.0296(9) 0.0306(10) 0.0299(10) 0.0063(8) -0.0161(8) 0.0029(8) C24 0.0444(12) 0.0377(11) 0.0351(11) -0.0041(9) -0.0263(10) 0.0147(10) C25 0.0463(14) 0.0458(15) 0.082(2) -0.0113(14) -0.0424(15) 0.0100(12) C26 0.0511(15) 0.0454(14) 0.0407(13) -0.0066(11) -0.0131(11) 0.0067(11) C27 0.099(4) 0.078(3) 0.088(3) -0.006(2) 0.011(3) 0.011(3) C28 0.085(3) 0.072(3) 0.100(3) -0.006(2) -0.040(3) 0.009(2) N1 0.0266(8) 0.0274(8) 0.0408(10) -0.0104(7) -0.0146(7) 0.0055(6) N2 0.149(5) 0.113(4) 0.120(4) -0.022(3) -0.031(4) -0.016(4) O1 0.0382(8) 0.0359(8) 0.0232(7) 0.0022(6) -0.0114(6) -0.0113(6) O2 0.0198(6) 0.0260(7) 0.0304(7) 0.0042(5) -0.0101(5) -0.0018(5) O3 0.0238(6) 0.0270(7) 0.0177(6) 0.0010(5) -0.0078(5) -0.0044(5) O4 0.0403(8) 0.0343(8) 0.0213(7) -0.0035(6) -0.0120(6) -0.0076(6) O5 0.0174(5) 0.0247(6) 0.0175(6) 0.0011(5) -0.0085(5) 0.0010(5) O6 0.0278(7) 0.0264(7) 0.0334(7) -0.0082(6) -0.0176(6) 0.0011(5) O7 0.0358(7) 0.0226(6) 0.0294(7) -0.0075(5) -0.0223(6) 0.0023(5) O8 0.0326(7) 0.0233(6) 0.0290(7) -0.0090(5) -0.0201(6) 0.0016(5) O9 0.0358(8) 0.0501(10) 0.0601(11) -0.0364(9) -0.0227(8) 0.0043(7) O10 0.0359(8) 0.0316(7) 0.0334(8) -0.0113(6) -0.0222(6) 0.0025(6) O11 0.0251(6) 0.0381(8) 0.0215(6) -0.0080(6) -0.0101(5) 0.0119(6) O12 0.0227(6) 0.0266(7) 0.0214(6) -0.0047(5) -0.0049(5) 0.0090(5) O13 0.0262(6) 0.0272(7) 0.0236(6) -0.0098(5) -0.0111(5) 0.0121(5) O14 0.0319(7) 0.0352(8) 0.0296(7) -0.0125(6) -0.0150(6) 0.0147(6) O15 0.0365(7) 0.0211(6) 0.0261(7) -0.0074(5) -0.0136(6) 0.0075(5) O16 0.0240(6) 0.0204(6) 0.0355(7) 0.0008(5) -0.0165(6) 0.0004(5) O17 0.0236(6) 0.0264(7) 0.0242(6) 0.0045(5) -0.0135(5) 0.0003(5) O18 0.0219(6) 0.0280(7) 0.0267(7) 0.0030(5) -0.0148(5) 0.0026(5) O19 0.0313(8) 0.0686(12) 0.0374(9) 0.0022(8) -0.0204(7) 0.0138(8) O20 0.0902(17) 0.0588(13) 0.0952(18) 0.0399(13) -0.0726(16) -0.0149(12) Zn1 0.02217(10) 0.01917(10) 0.02015(10) -0.00390(7) -0.01042(8) 0.00081(7) Zn2 0.01787(10) 0.02305(11) 0.01941(10) -0.00091(8) -0.01024(8) 0.00230(7) Zn3 0.01785(13) 0.01533(13) 0.01651(13) -0.00235(9) -0.00919(10) 0.00166(9) Zn4 0.01619(12) 0.01810(13) 0.01569(13) -0.00477(10) -0.00881(10) 0.00333(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 O2 1.249(2) . ? C1 O1 1.268(2) . ? C1 C2 1.474(3) . ? C2 C3 1.356(3) . ? C2 O3 1.369(2) . ? C3 C4 1.422(3) . ? C3 H3 0.9300 . ? C4 C5 1.353(3) . ? C4 H4 0.9300 . ? C5 O3 1.364(2) . ? C5 C6 1.482(3) . ? C6 O4 1.220(2) . ? C6 O5 1.308(2) . ? C7 O7 1.244(2) . ? C7 O6 1.271(2) . ? C7 C8 1.478(3) . ? C8 C9 1.353(3) . ? C8 O8 1.371(2) . ? C9 C10 1.428(3) . ? C9 H9 0.9300 . ? C10 C11 1.352(3) . ? C10 H10 0.9300 . ? C11 O8 1.369(2) . ? C11 C12 1.482(3) 2 ? C12 O9 1.225(3) . ? C12 O10 1.278(3) . ? C12 C11 1.482(3) 2 ? C13 O12 1.247(2) . ? C13 O11 1.269(2) . ? C13 C14 1.474(2) . ? C14 C15 1.355(3) . ? C14 O13 1.370(2) . ? C15 C16 1.423(3) . ? C15 H15 0.9300 . ? C16 C17 1.362(3) . ? C16 H16 0.9300 . ? C17 O13 1.359(2) . ? C17 C18 1.482(2) 1_456 ? C18 O15 1.243(2) . ? C18 O14 1.270(2) . ? C18 C17 1.482(3) 1_654 ? C19 O17 1.240(2) . ? C19 O16 1.269(2) . ? C19 C20 1.476(2) . ? C20 C21 1.356(3) . ? C20 O18 1.368(2) . ? C21 C22 1.423(3) . ? C21 H21 0.9300 . ? C22 C23 1.347(3) . ? C22 H22 0.9300 . ? C23 O18 1.354(2) . ? C23 C24 1.481(3) 2_565 ? C24 O19 1.229(3) . ? C24 O20 1.242(3) . ? C24 C23 1.481(3) 2_565 ? C24 Zn2 2.493(2) . ? C25 N1 1.474(3) . ? C25 H31A 0.9600 . ? C25 H31B 0.9600 . ? C25 H31C 0.9600 . ? C26 N1 1.472(3) . ? C26 H32A 0.9600 . ? C26 H32B 0.9600 . ? C26 H32C 0.9600 . ? C27 N2 1.410(7) . ? C27 H34A 0.9600 . ? C27 H34B 0.9600 . ? C27 H34C 0.9600 . ? C28 N2 1.460(7) . ? C28 H33A 0.9600 . ? C28 H33B 0.9600 . ? C28 H33C 0.9600 . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? O1 Zn1 1.9415(15) . ? O2 Zn3 2.1326(13) . ? O5 Zn2 2.0081(13) . ? O5 Zn4 2.1322(12) . ? O6 Zn2 1.9600(14) . ? O7 Zn4 2.0711(13) . ? O10 Zn1 1.9624(14) . ? O11 Zn2 1.9755(14) . ? O12 Zn4 2.0593(13) . ? O14 Zn1 1.9560(14) . ? O15 Zn3 2.0619(14) . ? O16 Zn1 1.9398(14) . ? O17 Zn3 2.1080(13) . ? O19 Zn2 2.1072(17) . ? O20 Zn2 2.238(2) . ? Zn3 O15 2.0619(14) 2_665 ? Zn3 O17 2.1080(13) 2_665 ? Zn3 O2 2.1326(13) 2_665 ? Zn4 O12 2.0593(13) 2_556 ? Zn4 O7 2.0711(13) 2_556 ? Zn4 O5 2.1322(12) 2_556 ? 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 C1 O1 125.04(18) . . ? O2 C1 C2 118.61(18) . . ? O1 C1 C2 116.30(17) . . ? C3 C2 O3 110.50(16) . . ? C3 C2 C1 132.57(18) . . ? O3 C2 C1 116.92(16) . . ? C2 C3 C4 106.23(18) . . ? C2 C3 H3 126.9 . . ? C4 C3 H3 126.9 . . ? C5 C4 C3 106.49(17) . . ? C5 C4 H4 126.8 . . ? C3 C4 H4 126.8 . . ? C4 C5 O3 110.61(16) . . ? C4 C5 C6 133.27(17) . . ? O3 C5 C6 115.98(16) . . ? O4 C6 O5 124.87(17) . . ? O4 C6 C5 121.29(17) . . ? O5 C6 C5 113.72(16) . . ? O7 C7 O6 127.80(18) . . ? O7 C7 C8 115.43(17) . . ? O6 C7 C8 116.76(16) . . ? C9 C8 O8 110.67(17) . . ? C9 C8 C7 131.70(18) . . ? O8 C8 C7 117.37(17) . . ? C8 C9 C10 106.08(19) . . ? C8 C9 H9 127.0 . . ? C10 C9 H9 127.0 . . ? C11 C10 C9 106.7(2) . . ? C11 C10 H10 126.7 . . ? C9 C10 H10 126.7 . . ? C10 C11 O8 110.39(17) . . ? C10 C11 C12 131.90(19) . 2 ? O8 C11 C12 117.59(18) . 2 ? O9 C12 O10 125.59(19) . . ? O9 C12 C11 118.3(2) . 2 ? O10 C12 C11 116.09(18) . 2 ? O12 C13 O11 125.61(17) . . ? O12 C13 C14 116.82(17) . . ? O11 C13 C14 117.57(16) . . ? C15 C14 O13 110.71(16) . . ? C15 C14 C13 132.01(17) . . ? O13 C14 C13 117.25(16) . . ? C14 C15 C16 106.33(18) . . ? C14 C15 H15 126.8 . . ? C16 C15 H15 126.8 . . ? C17 C16 C15 106.02(18) . . ? C17 C16 H16 127.0 . . ? C15 C16 H16 127.0 . . ? O13 C17 C16 110.91(17) . . ? O13 C17 C18 116.72(17) . 1_456 ? C16 C17 C18 132.34(18) . 1_456 ? O15 C18 O14 127.59(18) . . ? O15 C18 C17 116.68(17) . 1_654 ? O14 C18 C17 115.71(17) . 1_654 ? O17 C19 O16 127.39(17) . . ? O17 C19 C20 117.98(16) . . ? O16 C19 C20 114.62(16) . . ? C21 C20 O18 110.29(17) . . ? C21 C20 C19 133.64(17) . . ? O18 C20 C19 116.02(16) . . ? C20 C21 C22 106.01(19) . . ? C20 C21 H21 127.0 . . ? C22 C21 H21 127.0 . . ? C23 C22 C21 106.5(2) . . ? C23 C22 H22 126.8 . . ? C21 C22 H22 126.8 . . ? C22 C23 O18 110.85(17) . . ? C22 C23 C24 132.3(2) . 2_565 ? O18 C23 C24 116.82(19) . 2_565 ? O19 C24 O20 121.2(2) . . ? O19 C24 C23 120.8(2) . 2_565 ? O20 C24 C23 118.0(2) . 2_565 ? O19 C24 Zn2 57.59(12) . . ? O20 C24 Zn2 63.66(14) . . ? C23 C24 Zn2 178.26(18) 2_565 . ? N1 C25 H31A 109.5 . . ? N1 C25 H31B 109.5 . . ? H31A C25 H31B 109.5 . . ? N1 C25 H31C 109.5 . . ? H31A C25 H31C 109.5 . . ? H31B C25 H31C 109.5 . . ? N1 C26 H32A 109.5 . . ? N1 C26 H32B 109.5 . . ? H32A C26 H32B 109.5 . . ? N1 C26 H32C 109.5 . . ? H32A C26 H32C 109.5 . . ? H32B C26 H32C 109.5 . . ? N2 C27 H34A 109.5 . . ? N2 C27 H34B 109.5 . . ? H34A C27 H34B 109.5 . . ? N2 C27 H34C 109.5 . . ? H34A C27 H34C 109.5 . . ? H34B C27 H34C 109.5 . . ? N2 C28 H33A 109.5 . . ? N2 C28 H33B 109.5 . . ? H33A C28 H33B 109.5 . . ? N2 C28 H33C 109.5 . . ? H33A C28 H33C 109.5 . . ? H33B C28 H33C 109.5 . . ? C26 N1 C25 114.6(2) . . ? C26 N1 H1A 108.6 . . ? C25 N1 H1A 108.6 . . ? C26 N1 H1B 108.6 . . ? C25 N1 H1B 108.6 . . ? H1A N1 H1B 107.6 . . ? C27 N2 C28 115.8(5) . . ? C27 N2 H2A 108.3 . . ? C28 N2 H2A 108.3 . . ? C27 N2 H2B 108.3 . . ? C28 N2 H2B 108.3 . . ? H2A N2 H2B 107.4 . . ? C1 O1 Zn1 114.00(13) . . ? C1 O2 Zn3 132.17(13) . . ? C5 O3 C2 106.17(14) . . ? C6 O5 Zn2 112.74(11) . . ? C6 O5 Zn4 122.27(11) . . ? Zn2 O5 Zn4 103.22(6) . . ? C7 O6 Zn2 123.35(12) . . ? C7 O7 Zn4 134.79(13) . . ? C11 O8 C8 106.17(15) . . ? C12 O10 Zn1 113.37(13) . . ? C13 O11 Zn2 116.10(12) . . ? C13 O12 Zn4 128.45(12) . . ? C17 O13 C14 106.04(15) . . ? C18 O14 Zn1 124.42(13) . . ? C18 O15 Zn3 135.94(13) . . ? C19 O16 Zn1 123.47(12) . . ? C19 O17 Zn3 132.82(12) . . ? C23 O18 C20 106.34(15) . . ? C24 O19 Zn2 92.90(15) . . ? C24 O20 Zn2 86.53(17) . . ? O16 Zn1 O1 124.50(7) . . ? O16 Zn1 O14 109.57(6) . . ? O1 Zn1 O14 107.06(7) . . ? O16 Zn1 O10 106.96(6) . . ? O1 Zn1 O10 104.75(7) . . ? O14 Zn1 O10 101.59(6) . . ? O6 Zn2 O11 121.78(6) . . ? O6 Zn2 O5 105.01(6) . . ? O11 Zn2 O5 96.51(6) . . ? O6 Zn2 O19 123.07(7) . . ? O11 Zn2 O19 106.88(7) . . ? O5 Zn2 O19 96.31(6) . . ? O6 Zn2 O20 90.19(8) . . ? O11 Zn2 O20 91.24(9) . . ? O5 Zn2 O20 155.62(7) . . ? O19 Zn2 O20 59.31(7) . . ? O6 Zn2 C24 108.96(7) . . ? O11 Zn2 C24 99.85(7) . . ? O5 Zn2 C24 125.80(7) . . ? O19 Zn2 C24 29.50(8) . . ? O20 Zn2 C24 29.82(8) . . ? O15 Zn3 O15 180.0 . 2_665 ? O15 Zn3 O17 85.31(6) . 2_665 ? O15 Zn3 O17 94.69(6) 2_665 2_665 ? O15 Zn3 O17 94.69(6) . . ? O15 Zn3 O17 85.31(6) 2_665 . ? O17 Zn3 O17 180.00(8) 2_665 . ? O15 Zn3 O2 86.04(6) . 2_665 ? O15 Zn3 O2 93.96(6) 2_665 2_665 ? O17 Zn3 O2 98.27(5) 2_665 2_665 ? O17 Zn3 O2 81.73(5) . 2_665 ? O15 Zn3 O2 93.96(6) . . ? O15 Zn3 O2 86.04(6) 2_665 . ? O17 Zn3 O2 81.73(5) 2_665 . ? O17 Zn3 O2 98.27(5) . . ? O2 Zn3 O2 180.00(8) 2_665 . ? O12 Zn4 O12 180.0 2_556 . ? O12 Zn4 O7 86.72(6) 2_556 . ? O12 Zn4 O7 93.28(6) . . ? O12 Zn4 O7 93.28(6) 2_556 2_556 ? O12 Zn4 O7 86.72(6) . 2_556 ? O7 Zn4 O7 180.00(4) . 2_556 ? O12 Zn4 O5 91.40(5) 2_556 2_556 ? O12 Zn4 O5 88.60(5) . 2_556 ? O7 Zn4 O5 88.09(5) . 2_556 ? O7 Zn4 O5 91.91(5) 2_556 2_556 ? O12 Zn4 O5 88.60(5) 2_556 . ? O12 Zn4 O5 91.40(5) . . ? O7 Zn4 O5 91.91(5) . . ? O7 Zn4 O5 88.09(5) 2_556 . ? O5 Zn4 O5 180.00(5) 2_556 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.942 _refine_diff_density_min -0.955 _refine_diff_density_rms 0.080 # 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 0.000 -0.004 0.320 1056 175 ' ' _platon_squeeze_details ; The SQUEEZE routine of the program PLATON was used in order to eliminate the contribution of disordered solvents molecules, thereby a final model based only on the ordered part of the crystal structure was obtained. The SQUEEZE routine suggested that a total potential solvent area volume of 681.5 Ang^3^[31.1% of cell volume], and a void electron population of 109 per cell. Refinement after the SQUEEZE routine gave significantly improved R values. [R values before SQUEEZE] R1 = 0.0436 for >2sigma(I) data R1 = 0.0462, wR2 = 0.1469, GooF = S = 1.088 for all data ( 11299 data and 0 restraint / 583 parameters) ;