Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Bai, Guangcai' 'Cui, Chunming' 'Hao, Haijun' 'Noltemeyer, Mathias' 'Roesky, H. W.' 'Schmidt, Hans-Georg' _publ_contact_author_name 'Prof H W Roesky' _publ_contact_author_address ; Prof H W Roesky Institut fur Anorganische Chemie Universitat Gottingen Tammannstrasse 4 Gottingen 37077 GERMANY ; _publ_contact_author_email 'HROESKY@GWDG.DE' data_roe901x _database_code_CSD 155083 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H50 F2 N4 Zn2' _chemical_formula_weight 779.60 _chemical_melting_point ? _chemical_compound_source ? 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' 'F' 'F' 0.0171 0.0103 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.026(2) _cell_length_b 8.8051(12) _cell_length_c 17.309(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.240(11) _cell_angle_gamma 90.00 _cell_volume 1915.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_crystal_description blocks _exptl_crystal_colour none _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method ? _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.296 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'STOE AED2' _diffrn_measurement_method 'profile fit' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '90 min' _diffrn_standards_decay_% none _diffrn_reflns_number 6762 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.0657 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3381 _reflns_number_observed 3163 _reflns_observed_criterion >2sigma(I) _computing_data_collection DIF4 _computing_cell_refinement DIF4 _computing_data_reduction REDU4 _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0144P)^2^+0.5878P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3380 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_obs 0.0272 _refine_ls_wR_factor_all 0.0723 _refine_ls_wR_factor_obs 0.0702 _refine_ls_goodness_of_fit_all 1.113 _refine_ls_goodness_of_fit_obs 1.123 _refine_ls_restrained_S_all 1.116 _refine_ls_restrained_S_obs 1.123 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.545089(14) 0.42197(2) 0.077763(13) 0.02998(9) Uani 1 d . . F1 F 0.53982(8) 0.62949(11) 0.02942(7) 0.0379(3) Uani 1 d . . N1 N 0.68760(11) 0.3392(2) 0.12397(10) 0.0315(4) Uani 1 d . . N2 N 0.48468(11) 0.39578(15) 0.16875(10) 0.0284(3) Uani 1 d . . C1 C 0.72222(13) 0.3264(2) 0.20303(13) 0.0311(4) Uani 1 d . . C2 C 0.66061(14) 0.3559(2) 0.25669(13) 0.0331(4) Uani 1 d . . H2A H 0.69881(14) 0.3614(2) 0.31085(13) 0.040 Uiso 1 calc R . C3 C 0.55034(14) 0.3784(2) 0.24163(13) 0.0309(4) Uani 1 d . . C4 C 0.83524(14) 0.2717(2) 0.24007(15) 0.0416(5) Uani 1 d . . H4A H 0.8444(4) 0.1714(9) 0.2198(8) 0.062 Uiso 1 calc R . H4B H 0.8482(4) 0.2674(18) 0.2978(2) 0.062 Uiso 1 calc R . H4C H 0.88522(15) 0.3415(11) 0.2262(8) 0.062 Uiso 1 calc R . C5 C 0.5061(2) 0.3809(2) 0.31347(14) 0.0396(5) Uani 1 d . . H5A H 0.4645(9) 0.4726(8) 0.3126(4) 0.059 Uiso 1 calc R . H5B H 0.5641(2) 0.3791(16) 0.36187(14) 0.059 Uiso 1 calc R . H5C H 0.4611(9) 0.2928(8) 0.3124(4) 0.059 Uiso 1 calc R . C11 C 0.75250(13) 0.2781(2) 0.07596(13) 0.0352(4) Uani 1 d . . C12 C 0.82910(14) 0.3673(2) 0.05503(15) 0.0432(5) Uani 1 d . . C13 C 0.8949(2) 0.2984(3) 0.0135(2) 0.0529(6) Uani 1 d . . H13A H 0.9484(2) 0.3559(3) -0.0001(2) 0.063 Uiso 1 calc R . C14 C 0.8826(2) 0.1475(3) -0.0081(2) 0.0548(6) Uani 1 d . . H14A H 0.9285(2) 0.1024(3) -0.0353(2) 0.066 Uiso 1 calc R . C15 C 0.8035(2) 0.0626(3) 0.0100(2) 0.0489(6) Uani 1 d . . H15A H 0.7948(2) -0.0397(3) -0.0060(2) 0.059 Uiso 1 calc R . C16 C 0.73624(15) 0.1255(2) 0.05147(14) 0.0388(5) Uani 1 d . . C121 C 0.8406(2) 0.5339(3) 0.0765(2) 0.0606(7) Uani 1 d . . H12A H 0.7745(6) 0.5861(5) 0.0521(11) 0.091 Uiso 1 calc R . H12B H 0.8975(12) 0.5775(6) 0.0571(12) 0.091 Uiso 1 calc R . H12C H 0.8572(17) 0.5451(3) 0.1343(2) 0.091 Uiso 1 calc R . C161 C 0.6472(2) 0.0349(2) 0.0696(2) 0.0491(6) Uani 1 d . . H16A H 0.6523(8) 0.0404(16) 0.1264(2) 0.074 Uiso 1 calc R . H16B H 0.6527(8) -0.0702(5) 0.0543(10) 0.074 Uiso 1 calc R . H16C H 0.5794(2) 0.0761(13) 0.0396(8) 0.074 Uiso 1 calc R . C21 C 0.37249(13) 0.3834(2) 0.16125(12) 0.0303(4) Uani 1 d . . C22 C 0.32822(14) 0.2375(2) 0.15941(13) 0.0364(4) Uani 1 d . . C23 C 0.2202(2) 0.2263(3) 0.1551(2) 0.0469(5) Uani 1 d . . H23A H 0.1889(2) 0.1299(3) 0.1540(2) 0.056 Uiso 1 calc R . C24 C 0.1584(2) 0.3540(3) 0.1525(2) 0.0502(6) Uani 1 d . . H24A H 0.0858(2) 0.3444(3) 0.1504(2) 0.060 Uiso 1 calc R . C25 C 0.2031(2) 0.4962(3) 0.15288(15) 0.0452(5) Uani 1 d . . H25A H 0.1604(2) 0.5829(3) 0.15080(15) 0.054 Uiso 1 calc R . C26 C 0.31052(14) 0.5138(2) 0.15630(13) 0.0357(4) Uani 1 d . . C221 C 0.3955(2) 0.0975(2) 0.1641(2) 0.0481(6) Uani 1 d . . H22A H 0.3511(3) 0.0080(2) 0.1606(11) 0.072 Uiso 1 calc R . H22B H 0.4499(9) 0.0966(11) 0.2146(5) 0.072 Uiso 1 calc R . H22C H 0.4289(11) 0.0975(10) 0.1202(6) 0.072 Uiso 1 calc R . C261 C 0.3587(2) 0.6696(2) 0.1562(2) 0.0459(5) Uani 1 d . . H26A H 0.4149(10) 0.6835(8) 0.2051(5) 0.069 Uiso 1 calc R . H26B H 0.3042(4) 0.7461(2) 0.1531(11) 0.069 Uiso 1 calc R . H26C H 0.3880(12) 0.6792(7) 0.1104(6) 0.069 Uiso 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 0.02798(12) 0.03653(13) 0.0270(2) 0.00520(8) 0.01010(11) 0.00308(7) F1 0.0440(6) 0.0383(5) 0.0309(7) 0.0050(5) 0.0089(5) 0.0006(4) N1 0.0277(7) 0.0368(7) 0.0315(10) 0.0009(7) 0.0104(7) 0.0032(6) N2 0.0290(7) 0.0310(7) 0.0267(10) 0.0016(6) 0.0101(7) -0.0005(5) C1 0.0300(8) 0.0309(8) 0.0320(11) -0.0012(8) 0.0072(8) 0.0008(7) C2 0.0334(9) 0.0379(9) 0.0263(11) -0.0007(8) 0.0051(8) 0.0008(7) C3 0.0363(9) 0.0270(8) 0.0303(11) -0.0005(8) 0.0103(8) -0.0011(7) C4 0.0355(9) 0.0493(11) 0.0373(13) -0.0033(10) 0.0048(9) 0.0080(8) C5 0.0385(9) 0.0513(11) 0.0302(12) -0.0014(10) 0.0114(9) 0.0008(8) C11 0.0274(8) 0.0470(10) 0.0304(11) 0.0013(9) 0.0063(8) 0.0058(7) C12 0.0320(9) 0.0598(12) 0.0387(14) 0.0013(11) 0.0106(9) -0.0004(9) C13 0.0340(10) 0.086(2) 0.0419(15) 0.0092(13) 0.0154(10) 0.0037(10) C14 0.0486(12) 0.081(2) 0.0368(14) 0.0012(13) 0.0154(10) 0.0272(11) C15 0.0510(12) 0.0577(12) 0.0358(15) -0.0027(10) 0.0074(11) 0.0204(10) C16 0.0369(9) 0.0444(10) 0.0313(12) 0.0014(10) 0.0025(9) 0.0099(8) C121 0.0593(13) 0.0662(14) 0.064(2) -0.0036(14) 0.0296(13) -0.0203(11) C161 0.0481(11) 0.0414(10) 0.055(2) -0.0005(11) 0.0084(11) -0.0006(9) C21 0.0295(8) 0.0382(9) 0.0259(11) 0.0010(8) 0.0122(8) -0.0015(7) C22 0.0390(9) 0.0410(9) 0.0310(12) -0.0023(9) 0.0121(8) -0.0065(8) C23 0.0450(10) 0.0583(12) 0.0405(13) -0.0052(11) 0.0168(10) -0.0200(9) C24 0.0308(9) 0.0802(15) 0.0415(14) 0.0006(12) 0.0130(9) -0.0050(10) C25 0.0371(10) 0.0635(13) 0.0379(13) 0.0055(11) 0.0148(9) 0.0126(9) C26 0.0371(9) 0.0413(10) 0.0307(11) 0.0031(9) 0.0127(8) 0.0035(8) C221 0.0583(12) 0.0355(10) 0.055(2) -0.0030(10) 0.0219(12) -0.0081(9) C261 0.0505(11) 0.0366(10) 0.054(2) 0.0041(10) 0.0196(11) 0.0082(8) _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 F1 1.9473(12) 3_665 ? Zn1 N2 1.951(2) . ? Zn1 N1 1.9588(14) . ? Zn1 F1 2.0034(11) . ? Zn1 Zn1 2.9754(6) 3_665 ? F1 Zn1 1.9473(12) 3_665 ? N1 C1 1.328(3) . ? N1 C11 1.437(3) . ? N2 C3 1.334(3) . ? N2 C21 1.437(2) . ? C1 C2 1.402(3) . ? C1 C4 1.521(2) . ? C2 C3 1.405(2) . ? C3 C5 1.502(3) . ? C11 C12 1.391(3) . ? C11 C16 1.408(3) . ? C12 C13 1.394(3) . ? C12 C121 1.512(3) . ? C13 C14 1.379(4) . ? C14 C15 1.375(4) . ? C15 C16 1.386(3) . ? C16 C161 1.507(3) . ? C21 C26 1.393(3) . ? C21 C22 1.405(2) . ? C22 C23 1.394(3) . ? C22 C221 1.502(3) . ? C23 C24 1.377(3) . ? C24 C25 1.381(3) . ? C25 C26 1.393(3) . ? C26 C261 1.509(3) . ? 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 F1 Zn1 N2 119.55(5) 3_665 . ? F1 Zn1 N1 122.85(6) 3_665 . ? N2 Zn1 N1 99.58(7) . . ? F1 Zn1 F1 82.28(5) 3_665 . ? N2 Zn1 F1 117.92(5) . . ? N1 Zn1 F1 115.77(5) . . ? F1 Zn1 Zn1 41.85(3) 3_665 3_665 ? N2 Zn1 Zn1 129.65(4) . 3_665 ? N1 Zn1 Zn1 130.37(5) . 3_665 ? F1 Zn1 Zn1 40.43(3) . 3_665 ? Zn1 F1 Zn1 97.72(5) 3_665 . ? C1 N1 C11 118.18(14) . . ? C1 N1 Zn1 118.74(13) . . ? C11 N1 Zn1 122.80(13) . . ? C3 N2 C21 117.4(2) . . ? C3 N2 Zn1 118.86(12) . . ? C21 N2 Zn1 123.54(13) . . ? N1 C1 C2 124.6(2) . . ? N1 C1 C4 119.3(2) . . ? C2 C1 C4 116.0(2) . . ? C1 C2 C3 129.7(2) . . ? N2 C3 C2 124.2(2) . . ? N2 C3 C5 119.4(2) . . ? C2 C3 C5 116.4(2) . . ? C12 C11 C16 121.5(2) . . ? C12 C11 N1 120.7(2) . . ? C16 C11 N1 117.8(2) . . ? C11 C12 C13 118.0(2) . . ? C11 C12 C121 121.0(2) . . ? C13 C12 C121 121.0(2) . . ? C14 C13 C12 121.1(2) . . ? C15 C14 C13 120.1(2) . . ? C14 C15 C16 121.0(2) . . ? C15 C16 C11 118.2(2) . . ? C15 C16 C161 121.4(2) . . ? C11 C16 C161 120.4(2) . . ? C26 C21 C22 121.6(2) . . ? C26 C21 N2 120.1(2) . . ? C22 C21 N2 118.2(2) . . ? C23 C22 C21 117.9(2) . . ? C23 C22 C221 120.8(2) . . ? C21 C22 C221 121.3(2) . . ? C24 C23 C22 121.2(2) . . ? C23 C24 C25 119.9(2) . . ? C24 C25 C26 121.3(2) . . ? C25 C26 C21 118.0(2) . . ? C25 C26 C261 120.9(2) . . ? C21 C26 C261 121.0(2) . . ? _refine_diff_density_max 0.380 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.052 data_roe909b _database_code_CSD 155084 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H58 N4 Zn2 incl. benzene' _chemical_formula_weight 821.72 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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 16.941(5) _cell_length_b 20.576(3) _cell_length_c 24.918(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8686(3) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_crystal_description blocks _exptl_crystal_colour none _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3472 _exptl_absorpt_coefficient_mu 1.141 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.4622 _exptl_absorpt_correction_T_max 0.5993 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE AED2 four circle diffractometer' _diffrn_measurement_method 'profile fitted theta omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '90 min' _diffrn_standards_decay_% none _diffrn_reflns_number 3065 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.03 _reflns_number_total 1915 _reflns_number_gt 1699 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE DIF4' _computing_cell_refinement 'STOE DIF4' _computing_data_reduction 'STOE REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0374P)^2^+20.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1915 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0831 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.197348(19) 0.1250 0.1250 0.02578(14) Uani 1 2 d S . . N1 N 0.27320(10) 0.19385(8) 0.14347(7) 0.0243(4) Uani 1 1 d . . . C1 C 0.35086(12) 0.18319(10) 0.14207(8) 0.0259(4) Uani 1 1 d . . . C2 C 0.38574(17) 0.1250 0.1250 0.0280(6) Uani 1 2 d S . . H2A H 0.4418 0.1250 0.1250 0.034 Uiso 1 2 calc SR . . C3 C 0.40620(14) 0.23651(12) 0.15985(10) 0.0374(5) Uani 1 1 d . . . H3A H 0.3980 0.2751 0.1374 0.056 Uiso 1 1 calc R . . H3B H 0.4609 0.2217 0.1562 0.056 Uiso 1 1 calc R . . H3C H 0.3956 0.2474 0.1974 0.056 Uiso 1 1 calc R . . C11 C 0.24722(12) 0.25689(10) 0.16031(8) 0.0249(4) Uani 1 1 d . . . C12 C 0.23945(13) 0.30642(11) 0.12205(9) 0.0312(5) Uani 1 1 d . . . C13 C 0.21930(16) 0.36831(12) 0.13938(10) 0.0393(6) Uani 1 1 d . . . H13A H 0.2157 0.4027 0.1140 0.047 Uiso 1 1 calc R . . C14 C 0.20440(15) 0.38074(12) 0.19274(11) 0.0432(6) Uani 1 1 d . . . H14A H 0.1911 0.4235 0.2040 0.052 Uiso 1 1 calc R . . C15 C 0.20873(14) 0.33119(13) 0.22993(10) 0.0398(6) Uani 1 1 d . . . H15A H 0.1970 0.3399 0.2665 0.048 Uiso 1 1 calc R . . C16 C 0.23014(13) 0.26852(11) 0.21439(8) 0.0307(5) Uani 1 1 d . . . C121 C 0.25371(17) 0.29244(13) 0.06350(9) 0.0454(6) Uani 1 1 d . . . H12A H 0.2401 0.3309 0.0422 0.068 Uiso 1 1 calc R . . H12B H 0.2208 0.2557 0.0522 0.068 Uiso 1 1 calc R . . H12C H 0.3095 0.2816 0.0580 0.068 Uiso 1 1 calc R . . C161 C 0.23735(16) 0.21508(12) 0.25538(9) 0.0425(6) Uani 1 1 d . . . H16A H 0.2257 0.2325 0.2911 0.064 Uiso 1 1 calc R . . H16B H 0.2912 0.1977 0.2549 0.064 Uiso 1 1 calc R . . H16C H 0.1999 0.1803 0.2468 0.064 Uiso 1 1 calc R . . C21 C 0.3750 0.3089(2) 0.3750 0.0671(13) Uani 1 2 d S . . H21A H 0.3750 0.2627 0.3750 0.080 Uiso 1 2 calc SR . . C22 C 0.37497(18) 0.34182(18) 0.32768(14) 0.0682(9) Uani 1 1 d . . . H22A H 0.3749 0.3187 0.2947 0.082 Uiso 1 1 calc R . . H1 H 0.1250 0.1250 0.0740(13) 0.036(9) Uiso 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 Zn1 0.0183(2) 0.0229(2) 0.0361(2) -0.00091(14) 0.000 0.000 N1 0.0208(9) 0.0231(9) 0.0292(9) 0.0009(7) 0.0009(7) -0.0019(7) C1 0.0240(10) 0.0296(11) 0.0239(10) 0.0025(8) 0.0005(8) -0.0031(9) C2 0.0170(14) 0.0349(16) 0.0321(15) 0.0014(13) 0.000 0.000 C3 0.0265(11) 0.0357(12) 0.0499(14) -0.0048(11) -0.0008(11) -0.0061(10) C11 0.0204(10) 0.0232(10) 0.0312(10) 0.0003(8) 0.0001(8) -0.0030(8) C12 0.0303(11) 0.0302(11) 0.0331(11) 0.0042(9) 0.0001(9) -0.0029(10) C13 0.0424(13) 0.0267(12) 0.0488(14) 0.0062(10) -0.0029(11) 0.0002(10) C14 0.0441(15) 0.0291(12) 0.0564(16) -0.0090(11) -0.0016(12) 0.0042(11) C15 0.0385(13) 0.0455(14) 0.0353(12) -0.0115(11) 0.0023(10) -0.0004(11) C16 0.0291(11) 0.0344(12) 0.0285(10) -0.0001(9) -0.0003(9) -0.0019(10) C121 0.0603(17) 0.0441(15) 0.0318(12) 0.0100(11) 0.0037(12) 0.0028(13) C161 0.0511(15) 0.0466(15) 0.0298(12) 0.0073(11) 0.0011(11) -0.0042(12) C21 0.035(2) 0.046(2) 0.120(4) 0.000 0.003(3) 0.000 C22 0.0417(15) 0.091(2) 0.072(2) -0.0286(19) -0.0004(16) -0.0002(18) _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 1.9672(17) . ? Zn1 N1 1.9673(17) 8_544 ? Zn1 Zn1 2.4513(9) 14_445 ? N1 C1 1.334(3) . ? N1 C11 1.432(3) . ? C1 C2 1.401(2) . ? C1 C3 1.509(3) . ? C2 C1 1.401(2) 8_544 ? C11 C16 1.399(3) . ? C11 C12 1.402(3) . ? C12 C13 1.387(3) . ? C12 C121 1.507(3) . ? C13 C14 1.377(4) . ? C14 C15 1.380(4) . ? C15 C16 1.394(3) . ? C16 C161 1.506(3) . ? C21 C22 1.360(4) . ? C21 C22 1.360(4) 3 ? C22 C22 1.365(8) 2 ? 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 N1 98.43(10) . 8_544 ? N1 Zn1 Zn1 130.78(5) . 14_445 ? N1 Zn1 Zn1 130.78(5) 8_544 14_445 ? C1 N1 C11 117.35(17) . . ? C1 N1 Zn1 121.31(14) . . ? C11 N1 Zn1 121.33(13) . . ? N1 C1 C2 124.3(2) . . ? N1 C1 C3 119.04(19) . . ? C2 C1 C3 116.6(2) . . ? C1 C2 C1 130.1(3) . 8_544 ? C16 C11 C12 120.7(2) . . ? C16 C11 N1 120.05(18) . . ? C12 C11 N1 119.21(18) . . ? C13 C12 C11 118.6(2) . . ? C13 C12 C121 121.1(2) . . ? C11 C12 C121 120.3(2) . . ? C14 C13 C12 121.1(2) . . ? C13 C14 C15 120.1(2) . . ? C14 C15 C16 120.7(2) . . ? C15 C16 C11 118.7(2) . . ? C15 C16 C161 120.5(2) . . ? C11 C16 C161 120.8(2) . . ? C22 C21 C22 120.2(4) . 3 ? C21 C22 C22 119.9(2) . 2 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.286 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.058