Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Dr. Andrea Bencini' _publ_contact_author_address ; Department of Chemistry, POlo Scientifico, University of Florence via della Lastruccia 3 I-50019 Sesto Fiorentino, Firenze, Italy ; _publ_contact_author_email andrea.bencini@unifi.it _publ_section_title ; Encapsulation of metal cations and anions within the cavity of bis(1,4,7-triazacyclononane) receptors Authors: C.Bazzicalupi, A.Bencini, E.Faggi, A. Garau, C.Giorgi, V. Lippolis, A. Perra, B.Valtancoli ; loop_ _publ_author_name C.Bazzicalupi A.Bencini E.Faggi 'A. Garau' C.Giorgi V.Lippolis ; A.Perra ; B.Valtancoli data_[ZnL1](NO3)2_CH3NO2 _database_code_depnum_ccdc_archive 'CCDC 279362' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C19 H35 N7 Zn 2+), (N O3 -1)2, C H3 N O2' _chemical_formula_sum 'C20 H38 N10 O8 Zn' _chemical_formula_weight 611.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.620(6) _cell_length_b 10.998(8) _cell_length_c 13.319(7) _cell_angle_alpha 90.00 _cell_angle_beta 108.71(5) _cell_angle_gamma 90.00 _cell_volume 1334.7(14) _cell_formula_units_Z 2 _cell_measurement_temperature 170 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 1.839 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.83 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 170 _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur3-Oxford Diffraction' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6639 _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_sigmaI/netI 0.0915 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.85 _diffrn_reflns_theta_max 65.59 _reflns_number_total 3636 _reflns_number_gt 2261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD - Oxford Diffraction' _computing_cell_refinement 'CrysAlis Red - Oxford Diffraction' _computing_data_reduction 'CrysAlis Red - Oxford Diffraction' _computing_structure_solution 'SIR97 (Altomare 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 Ver. 1.01\b (Farrugia, 1997)' _computing_publication_material 'PARST93 (Nardelli, 1993)' _refine_special_details ; All the non hydrogen atoms were anisotropically refined while the hydrogen atoms were introduced in calculated position and their coordinates were refined according to the linked atoms.Desorder affects the nitrate anion and the solvent molecules which gives rise to high displacement parameters. In particular, the N21O3 nitrate occupies two different positions (population parameter 0.5) with a nitrogen and an oxygen atom sharing the same coordinates. Some degree of desorder also affects the ligand and therefore the pyridine unit has been refined as a rigid group. The present complex presents chirality. In this structure only one optical isomer is present. The value of the Flack's parameter at the end of refinement was 0.03(6). Flack's parameter and R1 values for the wrong enantiomer were 0.92(7) and 6.60, respectively. In the same crystallization batch, very poor quality crystals, belonging to the P21/n centric space group, were found which showed the presence of both enantiomers. 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^)+(0.1147P)^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 refU _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0013(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(6) _refine_ls_number_reflns 3636 _refine_ls_number_parameters 360 _refine_ls_number_restraints 73 _refine_ls_R_factor_all 0.1050 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1759 _refine_ls_wR_factor_gt 0.1521 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.017 _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 Zn Zn 0.07393(10) 0.38619(15) 0.29136(7) 0.0530(5) Uani 1 1 d . . . N3B N 0.0523(7) 0.4097(9) 0.1237(5) 0.049(2) Uani 1 1 d . . . HN3B H 0.1283 0.3716 0.1102 0.058 Uiso 1 1 calc R . . N3 N 0.0960(7) 0.3611(10) 0.4523(5) 0.053(3) Uani 1 1 d . . . H3 H 0.0035 0.3524 0.4555 0.064 Uiso 1 1 calc R . . N41 N -0.2037(9) 0.3305(14) 0.5601(7) 0.072(3) Uani 1 1 d . . . C4 C 0.3045(10) 0.2206(11) 0.4495(7) 0.054(3) Uani 1 1 d . . . H4A H 0.3889 0.2654 0.4935 0.065 Uiso 1 1 calc R . . H4B H 0.3279 0.1346 0.4584 0.065 Uiso 1 1 calc R . . N2A N -0.1851(7) 0.3924(15) 0.2125(5) 0.079(3) Uani 1 1 d . . . C4C C -0.2342(15) 0.5040(18) 0.2522(9) 0.089(5) Uani 1 1 d . . . H4CA H -0.2245 0.4945 0.3265 0.107 Uiso 1 1 calc R . . H4CB H -0.3366 0.5193 0.2132 0.107 Uiso 1 1 calc R . . O8 O -0.2863(8) 0.3054(9) 0.6127(6) 0.101(3) Uani 1 1 d . . . C4A C 0.4010(10) 0.3199(9) 0.3201(7) 0.047(3) Uani 1 1 d . . . H4AA H 0.3751 0.3401 0.2455 0.057 Uiso 1 1 calc R . . H4AB H 0.4860 0.2669 0.3377 0.057 Uiso 1 1 calc R . . N2 N 0.2782(8) 0.2538(8) 0.3379(6) 0.047(2) Uani 1 1 d . . . O14 O -0.1924(8) 0.4344(10) 0.5248(6) 0.081(3) Uani 1 1 d . . . C6 C 0.1618(11) 0.4656(13) 0.5217(8) 0.068(4) Uani 1 1 d . . . H6A H 0.1684 0.4467 0.5942 0.082 Uiso 1 1 calc R . . H6B H 0.0994 0.5364 0.4995 0.082 Uiso 1 1 calc R . . C4B C -0.2172(7) 0.3911(19) 0.0975(6) 0.083(4) Uani 1 1 d . . . H4BA H -0.2485 0.4717 0.0699 0.099 Uiso 1 1 calc R . . H4BB H -0.2980 0.3356 0.0665 0.099 Uiso 1 1 calc R . . C6B C 0.0516(10) 0.5415(11) 0.0940(6) 0.054(3) Uani 1 1 d . . . H6BA H -0.0446 0.5629 0.0460 0.065 Uiso 1 1 calc R . . H6BB H 0.1224 0.5543 0.0571 0.065 Uiso 1 1 calc R . . C5C C -0.1379(11) 0.6134(13) 0.2378(8) 0.074(4) Uani 1 1 d . . . H5CA H -0.1715 0.6388 0.1642 0.088 Uiso 1 1 calc R . . H5CB H -0.1510 0.6812 0.2805 0.088 Uiso 1 1 calc R . . N21 N 0.3727(12) 0.3105(14) 0.0254(8) 0.085(3) Uani 0.50 1 d PU . . O55' O 0.3727(12) 0.3105(14) 0.0254(8) 0.085(3) Uani 0.50 1 d P . . N3A N 0.3169(8) 0.4982(8) 0.4033(7) 0.052(2) Uani 1 1 d . . . H22A H 0.3217 0.5771 0.3866 0.050 Uiso 1 1 d . . . C6A C 0.3154(11) 0.4940(12) 0.5162(8) 0.068(3) Uani 1 1 d . . . H6AA H 0.3480 0.5717 0.5500 0.082 Uiso 1 1 calc R . . H6AB H 0.3836 0.4322 0.5549 0.082 Uiso 1 1 calc R . . N25 N 0.5272(14) 0.2828(13) -0.2053(11) 0.105(4) Uani 1 1 d U . . C5A C 0.4420(9) 0.4358(8) 0.3846(8) 0.049(3) Uani 1 1 d . . . H5AA H 0.5138 0.4164 0.4525 0.059 Uiso 1 1 calc R . . H5AB H 0.4879 0.4912 0.3481 0.059 Uiso 1 1 calc R . . C3 C 0.2363(11) 0.1464(10) 0.2678(7) 0.062(3) Uani 1 1 d . . . H3A H 0.2494 0.1656 0.2003 0.074 Uiso 1 1 calc R . . H3B H 0.3022 0.0799 0.2992 0.074 Uiso 1 1 calc R . . C5B C -0.0841(9) 0.3521(13) 0.0626(6) 0.076(5) Uani 1 1 d . . . H5BA H -0.0725 0.2646 0.0696 0.091 Uiso 1 1 calc R . . H5BB H -0.1046 0.3723 -0.0117 0.091 Uiso 1 1 calc R . . C3B C -0.2360(14) 0.2779(19) 0.2491(10) 0.112(7) Uani 1 1 d . . . H3BA H -0.2228 0.2838 0.3242 0.135 Uiso 1 1 calc R . . H3BB H -0.3398 0.2666 0.2118 0.135 Uiso 1 1 calc R . . C5 C 0.1710(12) 0.2468(14) 0.4889(8) 0.072(4) Uani 1 1 d . . . H5A H 0.1008 0.1810 0.4657 0.086 Uiso 1 1 calc R . . H5B H 0.2052 0.2468 0.5658 0.086 Uiso 1 1 calc R . . C6C C 0.0894(11) 0.6250(11) 0.1920(7) 0.064(3) Uani 1 1 d . . . H6CA H 0.1949 0.6258 0.2263 0.077 Uiso 1 1 calc R . . H6CB H 0.0584 0.7074 0.1697 0.077 Uiso 1 1 calc R . . O41 O 0.3876(16) 0.3987(18) 0.0744(11) 0.074(4) Uani 0.50 1 d P . . O54 O 0.4265(16) 0.265(2) -0.0256(13) 0.101(7) Uani 0.50 1 d P . . N21' N 0.285(2) 0.2342(14) 0.0312(10) 0.134(8) Uani 0.50 1 d P . . O55 O 0.285(2) 0.2342(14) 0.0312(10) 0.134(8) Uani 0.50 1 d P . . O56 O 0.5899(10) 0.3842(15) -0.1735(7) 0.124(3) Uani 1 1 d U . . O57 O -0.1282(9) 0.2472(9) 0.5416(6) 0.081(2) Uani 1 1 d . . . O58 O 0.2015(14) 0.252(2) 0.0165(15) 0.043(5) Uani 0.50 1 d P . . O59 O 0.3799(16) 0.1372(17) 0.0451(12) 0.082(6) Uani 0.50 1 d P . . N1 N -0.0072(8) 0.1986(6) 0.2572(5) 0.065(3) Uani 1 1 d GU . . C7 C 0.0868(6) 0.1062(7) 0.2486(5) 0.062(3) Uani 1 1 d GU . . C2 C 0.0311(9) -0.0083(6) 0.2132(6) 0.082(4) Uani 1 1 d GU . . H2 H 0.0940 -0.0701 0.2075 0.098 Uiso 1 1 calc R . . C1 C -0.1187(10) -0.0303(7) 0.1866(6) 0.095(4) Uani 1 1 d GU . . H1 H -0.1559 -0.1069 0.1629 0.114 Uiso 1 1 calc R . . C2B C -0.2127(7) 0.0621(9) 0.1952(6) 0.097(4) Uani 1 1 d GU . . H2B H -0.3129 0.0473 0.1773 0.117 Uiso 1 1 calc R . . C7B C -0.1570(7) 0.1766(7) 0.2305(6) 0.076(4) Uani 1 1 d GU . . N3C N 0.0170(9) 0.5836(9) 0.2681(6) 0.057(3) Uani 1 1 d . . . H3C H 0.0622 0.6217 0.3308 0.068 Uiso 1 1 calc R . . O40 O 0.4446(13) 0.2545(13) -0.2807(9) 0.169(5) Uani 1 1 d U . . C50 C 0.5956(16) 0.1875(16) -0.1297(14) 0.132(6) Uani 1 1 d U . . H50A H 0.5369 0.1719 -0.0849 0.050 Uiso 1 1 calc R . . H50B H 0.6919 0.2131 -0.0871 0.050 Uiso 1 1 calc R . . H50C H 0.6031 0.1146 -0.1673 0.050 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 Zn 0.0369(6) 0.0949(11) 0.0287(6) -0.0152(8) 0.0127(4) -0.0196(8) N3B 0.037(4) 0.076(8) 0.038(4) 0.003(5) 0.018(3) -0.014(4) N3 0.028(3) 0.097(8) 0.031(4) -0.009(5) 0.007(3) -0.006(5) N41 0.025(4) 0.153(12) 0.039(5) 0.023(6) 0.011(4) 0.024(6) C4 0.041(5) 0.085(9) 0.035(5) -0.004(5) 0.012(4) -0.025(5) N2A 0.033(4) 0.177(10) 0.026(3) 0.000(8) 0.009(3) -0.038(8) C4C 0.060(9) 0.188(17) 0.033(6) 0.002(9) 0.033(6) 0.003(10) O8 0.049(4) 0.205(10) 0.061(5) 0.053(5) 0.032(4) 0.036(5) C4A 0.043(5) 0.059(7) 0.044(5) -0.009(5) 0.020(5) -0.021(5) N2 0.055(5) 0.057(6) 0.033(4) -0.014(4) 0.018(4) -0.027(4) O14 0.055(5) 0.126(10) 0.055(5) 0.021(5) 0.010(4) 0.025(5) C6 0.044(6) 0.126(11) 0.036(6) -0.034(6) 0.014(5) -0.002(6) C4B 0.024(4) 0.193(12) 0.030(4) -0.018(10) 0.007(3) -0.001(9) C6B 0.048(6) 0.090(10) 0.028(5) -0.012(5) 0.016(4) 0.004(5) C5C 0.051(7) 0.144(13) 0.029(6) 0.004(7) 0.017(5) 0.027(7) N21 0.081(6) 0.094(7) 0.075(6) -0.003(5) 0.019(5) 0.024(5) O55' 0.081(6) 0.094(7) 0.075(6) -0.003(5) 0.019(5) 0.024(5) N3A 0.037(5) 0.058(6) 0.061(5) -0.003(5) 0.016(4) 0.001(4) C6A 0.056(7) 0.098(10) 0.040(6) -0.019(6) 0.001(5) -0.006(6) N25 0.093(7) 0.097(8) 0.116(8) 0.003(7) 0.022(6) -0.045(6) C5A 0.029(5) 0.056(8) 0.062(6) 0.003(5) 0.014(4) -0.017(4) C3 0.076(7) 0.068(8) 0.037(5) -0.018(5) 0.013(5) -0.031(6) C5B 0.054(5) 0.149(14) 0.025(4) -0.024(6) 0.013(4) -0.056(7) C3B 0.043(8) 0.25(2) 0.041(7) -0.021(11) 0.012(6) -0.072(11) C5 0.054(7) 0.143(13) 0.025(5) -0.012(7) 0.022(5) -0.037(8) C6C 0.062(7) 0.088(9) 0.037(5) -0.004(5) 0.009(5) 0.001(6) O41 0.103(11) 0.051(12) 0.073(9) -0.019(11) 0.034(8) -0.013(10) O54 0.055(9) 0.19(2) 0.085(11) -0.042(12) 0.063(9) -0.049(11) N21' 0.26(2) 0.069(12) 0.033(6) -0.003(6) -0.009(12) -0.042(17) O55 0.26(2) 0.069(12) 0.033(6) -0.003(6) -0.009(12) -0.042(17) O56 0.124(6) 0.142(7) 0.093(5) 0.012(7) 0.018(4) -0.042(7) O57 0.076(5) 0.109(8) 0.070(5) 0.024(5) 0.037(4) 0.006(5) O58 0.026(6) 0.072(12) 0.029(9) -0.005(8) 0.006(6) 0.025(8) O59 0.082(10) 0.087(13) 0.089(11) 0.063(10) 0.044(9) 0.059(10) N1 0.060(5) 0.107(7) 0.030(4) 0.000(5) 0.016(4) -0.043(5) C7 0.080(7) 0.071(7) 0.031(5) -0.009(5) 0.012(5) -0.046(6) C2 0.112(8) 0.090(8) 0.041(5) -0.003(5) 0.022(5) -0.039(6) C1 0.110(8) 0.110(8) 0.058(6) -0.012(6) 0.019(6) -0.071(7) C2B 0.093(7) 0.126(9) 0.073(7) -0.012(6) 0.026(6) -0.071(7) C7B 0.069(7) 0.118(9) 0.051(6) -0.012(6) 0.031(6) -0.056(7) N3C 0.042(5) 0.098(8) 0.029(4) -0.016(5) 0.010(4) 0.013(5) O40 0.156(8) 0.188(9) 0.112(7) 0.055(7) -0.030(6) -0.091(7) C50 0.116(9) 0.108(9) 0.149(10) -0.026(8) 0.009(8) 0.014(8) _geom_special_details ; Weighted least-squares planes through the starred atoms (Nardelli, Musatti, Domiano & Andreetti Ric.Sci.(1965),15(II-A),807). Equation of the plane: m1*X+m2*Y+m3*Z=d Plane 1 m1 = 0.37888(0.00218) m2 = 0.01282(0.00238) m3 = -0.92536(0.00091) D = -3.43126(0.00987) Atom d s d/s (d/s)**2 N1 * 0.0137 0.0065 2.090 4.367 N2A * -0.0119 0.0063 -1.881 3.536 N3C * 0.0119 0.0082 1.460 2.131 N2 * -0.0105 0.0072 -1.451 2.106 Zn -0.1177 0.0010 -116.989 13686.417 #=========== Sum((d/s)**2) for starred atoms 12.141 Chi-squared at 95% for 1 degrees of freedom: 3.84 The group of atoms deviates significantly from planarity Weighted least-squares lines through the starred atoms (Schoemaker,Waser,Marsh & Bergman,Acta Cryst.(1959).12,600) m1,m2,m3 are the direction cosines referred to the X,Y,Z orthogonal axes. X0,Y0,Z0 are the coordinates of the centroid of the set of atoms. Equation of the line: (X-X0)/m1=(Y-Y0)/m2=(Z-Z0)/m3 Line 1 m1 = -0.22893(0.00225) X0 = -0.51743(0.00487) m2 = -0.12443(0.00328) Y0 = 4.23879(0.00721) m3 = 0.96546(0.00062) Z0 = 3.63318(0.00451) Atom d s d/s (d/s)**2 N3B * 0.0000 0.0117 0.000 0.000 N3 * 0.0000 0.0127 0.000 0.000 #=========== Sum((d/s)**2) for starred atoms 0.000 Angles formed by lines and normals to planes Line - plane angle (s.u.) angle (s.u.) 1 1 10.97( 0.20) 169.03( 0.20) 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 Zn N3 2.103(7) . ? Zn N3B 2.190(6) . ? Zn N1 2.201(6) . ? Zn N3C 2.236(10) . ? Zn N2 2.363(9) . ? Zn N2A 2.374(7) . ? N3B C5B 1.449(10) . ? N3B C6B 1.502(13) . ? N3 C5 1.454(15) . ? N3 C6 1.483(14) . ? N41 O57 1.243(13) . ? N41 O14 1.253(12) . ? N41 O8 1.247(11) . ? C4 N2 1.471(11) . ? C4 C5 1.562(13) . ? N2A C4B 1.462(10) . ? N2A C4C 1.47(2) . ? N2A C3B 1.49(2) . ? C4C C5C 1.57(2) . ? C4A N2 1.470(11) . ? C4A C5A 1.517(12) . ? N2 C3 1.479(12) . ? C6 C6A 1.534(14) . ? C4B C5B 1.556(12) . ? C6B C6C 1.540(13) . ? C5C N3C 1.451(13) . ? N21 N21' 1.211(19) . ? N21 O41 1.152(18) . ? N21 O54 1.098(16) . ? N21 O58 1.73(2) . ? N3A C5A 1.474(11) . ? N3A C6A 1.509(13) . ? N25 O40 1.107(13) . ? N25 O56 1.274(18) . ? N25 C50 1.456(19) . ? C3 C7 1.447(10) . ? C3B C7B 1.41(2) . ? C6C N3C 1.475(12) . ? O54 N21' 1.79(2) . ? O54 O59 1.82(3) . ? N21' O58 0.79(2) . ? N21' O59 1.38(2) . ? N1 C7 1.3899 . ? N1 C7B 1.3901 . ? C7 C2 1.3900 . ? C2 C1 1.3900 . ? C1 C2B 1.3900 . ? C2B C7B 1.3900 . ? 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 Zn N3B 179.2(4) . . ? N3 Zn N1 90.0(3) . . ? N3B Zn N1 89.4(3) . . ? N3 Zn N3C 102.0(3) . . ? N3B Zn N3C 78.8(3) . . ? N1 Zn N3C 145.7(3) . . ? N3 Zn N2 81.3(3) . . ? N3B Zn N2 98.0(3) . . ? N1 Zn N2 71.7(3) . . ? N3C Zn N2 141.3(3) . . ? N3 Zn N2A 101.7(2) . . ? N3B Zn N2A 78.6(2) . . ? N1 Zn N2A 71.5(4) . . ? N3C Zn N2A 74.6(5) . . ? N2 Zn N2A 143.1(4) . . ? C5B N3B C6B 110.3(8) . . ? C5B N3B Zn 107.1(5) . . ? C6B N3B Zn 111.9(5) . . ? C5 N3 C6 113.2(8) . . ? C5 N3 Zn 109.4(6) . . ? C6 N3 Zn 114.6(7) . . ? O57 N41 O14 118.1(10) . . ? O57 N41 O8 117.8(13) . . ? O14 N41 O8 124.1(12) . . ? N2 C4 C5 113.6(8) . . ? C4B N2A C4C 113.6(13) . . ? C4B N2A C3B 110.7(12) . . ? C4C N2A C3B 114.2(8) . . ? C4B N2A Zn 107.6(4) . . ? C4C N2A Zn 106.1(7) . . ? C3B N2A Zn 103.9(8) . . ? N2A C4C C5C 109.0(9) . . ? N2 C4A C5A 113.7(7) . . ? C3 N2 C4 111.3(8) . . ? C3 N2 C4A 111.3(7) . . ? C4 N2 C4A 113.5(7) . . ? C3 N2 Zn 106.9(6) . . ? C4 N2 Zn 106.1(6) . . ? C4A N2 Zn 107.2(6) . . ? N3 C6 C6A 110.7(7) . . ? N2A C4B C5B 113.5(7) . . ? N3B C6B C6C 111.9(8) . . ? N3C C5C C4C 112.8(10) . . ? N21' N21 O41 120.6(16) . . ? N21' N21 O54 101.5(18) . . ? O41 N21 O54 137.5(19) . . ? N21' N21 O58 23.5(13) . . ? O41 N21 O58 106.9(12) . . ? O54 N21 O58 114.5(14) . . ? C5A N3A C6A 115.0(8) . . ? N3A C6A C6 111.7(8) . . ? O40 N25 O56 132.4(15) . . ? O40 N25 C50 117.3(15) . . ? O56 N25 C50 109.8(13) . . ? N3A C5A C4A 114.1(7) . . ? C7 C3 N2 114.2(8) . . ? N3B C5B C4B 113.3(9) . . ? C7B C3B N2A 111.0(11) . . ? N3 C5 C4 114.9(9) . . ? N3C C6C C6B 111.3(9) . . ? N21 O54 N21' 41.5(10) . . ? N21 O54 O59 77.9(12) . . ? N21' O54 O59 44.8(8) . . ? O58 N21' N21 119(3) . . ? O58 N21' O59 144(3) . . ? N21 N21' O59 96(2) . . ? O58 N21' O54 134(3) . . ? N21 N21' O54 37.0(11) . . ? O59 N21' O54 68.9(14) . . ? N21' O58 N21 38(2) . . ? N21' O59 O54 66.3(13) . . ? C7 N1 C7B 120.0 . . ? C7 N1 Zn 120.4(4) . . ? C7B N1 Zn 119.1(4) . . ? N1 C7 C2 120.0 . . ? N1 C7 C3 113.5(7) . . ? C2 C7 C3 126.1(7) . . ? C1 C2 C7 120.0 . . ? C2 C1 C2B 120.0 . . ? C7B C2B C1 120.0 . . ? C2B C7B N1 120.0 . . ? C2B C7B C3B 127.0(7) . . ? N1 C7B C3B 112.9(7) . . ? C5C N3C C6C 114.1(8) . . ? C5C N3C Zn 116.2(8) . . ? C6C N3C Zn 104.3(6) . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 65.59 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 0.781 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.082 #===END