Supplementary information (ESI) for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 # SUBMISSION DETAILS _publ_contact_author_name 'Prof. Chun-Hua Yan' _publ_contact_author_address ; State Key Lab of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Lab on Rare Earth Materials and Bioinorganic Chemistry, Peking University, Beijing 100871, China ; _publ_contact_author_email yan@pku.edu.cn _publ_contact_author_phone 86-(10)-62754179 _publ_contact_author_fax 86-(10)-62754179 _publ_requested_category FO _publ_section_title ; The crystal structures of four azido bridged Zn(II) complexes based on open-chain diazine Schiff-base ligands ; loop_ _publ_author_name _publ_author_address 'Yan-Feng Yue.' ; State Key Laboratory of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Laboratory in Rare Earth Materials and Bioinorganic Chemistry Peking University Beijing 100871 China ; 'En-Qing Gao.' ; Shanghai Key Lab of Green Chemistry and Chemical Process Greening East China Normal University Shanghai 200062 China ; 'Chen-Jie Fang.' ; State Key Laboratory of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Laboratory in Rare Earth Materials and Bioinorganic Chemistry Peking University Beijing 100871 China ; 'Tao Zheng.' ; State Key Laboratory of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Laboratory in Rare Earth Materials and Bioinorganic Chemistry Peking University Beijing 100871 China ; 'Jue Liang.' ; State Key Laboratory of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Laboratory in Rare Earth Materials and Bioinorganic Chemistry Peking University Beijing 100871 China ; ; Chun-Hua Yan ; ; State Key Laboratory of Rare Earth Materials Chemistry and Applications & PKU-HKU Joint Laboratory in Rare Earth Materials and Bioinorganic Chemistry Peking University Beijing 100871 China ; #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 641454' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H106 N102 O17 Zn17' _chemical_formula_weight 3735.84 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 13.5903(4) _cell_length_b 15.1186(6) _cell_length_c 18.8621(7) _cell_angle_alpha 101.383(2) _cell_angle_beta 99.6841(19) _cell_angle_gamma 95.3548(17) _cell_volume 3712.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 90474 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 24.407 _exptl_crystal_description Block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1874 _exptl_absorpt_coefficient_mu 2.775 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.466 _exptl_absorpt_correction_T_max 0.578 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _exptl_special_details ; Problems: _diffrn_reflns_theta_full (too) Low 23.37 Deg. The value of sine(theta_max)/wavelength is less than 0.5 Response: The weak diffraction of the crystals even at low temperature results in limited resolution Problems: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.90 Ratio Large Non-Solvent N Ueq(max)/Ueq(min) ... 10.00 Ratio Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.72 Ratio Check Low Ueq as Compared to Neighbors for N23 Check Low Ueq as Compared to Neighbors for N26 Check Low Ueq as Compared to Neighbors for N50' Response: These arise from the heavy disorder in azido ligand and the presence of terminal methyl groups in the structure Problem: Isotropic non-H Atoms in Main Residue(s) 2 Response: The disordered N50 and N51 atoms are refined isotropically to avoid non-positive definite and very large ADPs Problems: Short Inter D...A Contact O9 N45' 2.26 Ang. Short Inter D...A Contact O4 O7 2.65 Ang. Short Inter D...A Contact O7 O9 2.69 Ang. Response: The short inter D...A contact distances are due to the limited quality of the data set and the disorder problem. ; _diffrn_ambient_temperature 293(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 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46848 _diffrn_reflns_av_R_equivalents 0.1041 _diffrn_reflns_av_sigmaI/netI 0.0971 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 23.37 _reflns_number_total 10643 _reflns_number_gt 6458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0962P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10643 _refine_ls_number_parameters 964 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1046 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1666 _refine_ls_wR_factor_gt 0.1474 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.003 _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 0.0000 0.5000 0.5000 0.0307(3) Uani 1 2 d S . . Zn2 Zn -0.12985(7) 0.39860(7) 0.59652(5) 0.0327(3) Uani 1 1 d . . . Zn3 Zn 0.01962(7) 0.58659(6) 0.67374(5) 0.0316(3) Uani 1 1 d . . . Zn4 Zn 0.15288(7) 0.68921(6) 0.57773(5) 0.0323(3) Uani 1 1 d . . . Zn5 Zn -0.08291(8) 0.46194(7) 0.78279(5) 0.0346(3) Uani 1 1 d . . . Zn6 Zn 0.12518(7) 0.80567(7) 0.74607(5) 0.0337(3) Uani 1 1 d . . . Zn7 Zn 0.32513(8) 0.76951(7) 0.48614(6) 0.0364(3) Uani 1 1 d . A . Zn8 Zn 0.39007(9) 0.93949(8) 0.97187(6) 0.0529(3) Uani 1 1 d . . . Zn9 Zn -0.33586(11) 0.53488(11) 0.94584(8) 0.0774(5) Uani 1 1 d . . . C1 C -0.0247(8) 0.9463(6) 0.7510(5) 0.048(3) Uani 1 1 d . . . H1A H -0.0627 0.9055 0.7099 0.058 Uiso 1 1 calc R . . C2 C -0.0607(9) 1.0265(8) 0.7764(6) 0.070(3) Uani 1 1 d . . . H2A H -0.1211 1.0409 0.7531 0.084 Uiso 1 1 calc R . . C3 C -0.0015(10) 1.0854(8) 0.8394(8) 0.092(5) Uani 1 1 d . . . H3A H -0.0220 1.1406 0.8588 0.110 Uiso 1 1 calc R . . C4 C 0.0870(9) 1.0605(8) 0.8717(7) 0.084(4) Uani 1 1 d . . . H4A H 0.1261 1.0985 0.9139 0.101 Uiso 1 1 calc R . . C5 C 0.1176(7) 0.9804(6) 0.8421(5) 0.045(2) Uani 1 1 d . . . C6 C 0.2117(7) 0.9479(6) 0.8750(5) 0.043(2) Uani 1 1 d . . . C7 C 0.3313(7) 0.7522(7) 0.8488(5) 0.042(2) Uani 1 1 d . . . C8 C 0.2870(6) 0.6838(6) 0.7796(4) 0.031(2) Uani 1 1 d . . . C9 C 0.4192(7) 0.7240(7) 0.8967(5) 0.057(3) Uani 1 1 d . . . H9A H 0.4432 0.7712 0.9401 0.085 Uiso 1 1 calc R . . H9B H 0.4725 0.7144 0.8695 0.085 Uiso 1 1 calc R . . H9C H 0.3976 0.6687 0.9106 0.085 Uiso 1 1 calc R . . C10 C 0.3276(7) 0.5949(6) 0.7636(5) 0.044(2) Uani 1 1 d . . . H10A H 0.2913 0.5590 0.7172 0.066 Uiso 1 1 calc R . . H10B H 0.3200 0.5628 0.8019 0.066 Uiso 1 1 calc R . . H10C H 0.3977 0.6058 0.7615 0.066 Uiso 1 1 calc R . . C11 C 0.0637(8) 0.3605(7) 0.8708(5) 0.049(3) Uani 1 1 d . . . H11A H 0.0984 0.3576 0.8321 0.059 Uiso 1 1 calc R . . C12 C 0.0999(8) 0.3209(7) 0.9278(5) 0.055(3) Uani 1 1 d . . . H12A H 0.1584 0.2933 0.9287 0.066 Uiso 1 1 calc R . . C13 C 0.0452(9) 0.3238(7) 0.9839(6) 0.063(3) Uani 1 1 d . . . H13A H 0.0667 0.2965 1.0228 0.076 Uiso 1 1 calc R . . C14 C -0.0400(8) 0.3661(7) 0.9834(5) 0.049(3) Uani 1 1 d . . . H14A H -0.0763 0.3675 1.0211 0.059 Uiso 1 1 calc R . . C15 C -0.0705(7) 0.4070(6) 0.9242(5) 0.043(2) Uani 1 1 d . . . C16 C -0.1613(7) 0.4556(6) 0.9156(5) 0.040(2) Uani 1 1 d . . . C17 C -0.2884(7) 0.5728(7) 0.7951(5) 0.046(2) Uani 1 1 d . . . C18 C -0.2420(7) 0.5760(6) 0.7292(5) 0.044(2) Uani 1 1 d . . . C19 C -0.3819(8) 0.6184(8) 0.7968(6) 0.073(4) Uani 1 1 d . . . H19A H -0.4066 0.6134 0.8408 0.110 Uiso 1 1 calc R . . H19B H -0.4324 0.5893 0.7545 0.110 Uiso 1 1 calc R . . H19C H -0.3665 0.6814 0.7961 0.110 Uiso 1 1 calc R . . C20 C -0.2810(9) 0.6302(10) 0.6761(7) 0.091(5) Uani 1 1 d . . . H20A H -0.2428 0.6250 0.6374 0.137 Uiso 1 1 calc R . . H20B H -0.2751 0.6928 0.7009 0.137 Uiso 1 1 calc R . . H20C H -0.3505 0.6079 0.6555 0.137 Uiso 1 1 calc R . . C21 C 0.5440(7) 0.7144(7) 0.4995(5) 0.054(3) Uani 1 1 d . . . H21A H 0.5210 0.6694 0.5223 0.065 Uiso 1 1 calc R . . C22 C 0.6383(8) 0.7163(8) 0.4859(6) 0.068(3) Uani 1 1 d . . . H22A H 0.6790 0.6736 0.4988 0.081 Uiso 1 1 calc R . . C23 C 0.6729(8) 0.7830(9) 0.4523(7) 0.077(4) Uani 1 1 d . . . H23A H 0.7380 0.7861 0.4430 0.092 Uiso 1 1 calc R . . C24 C 0.6114(8) 0.8451(7) 0.4324(6) 0.061(3) Uani 1 1 d . . . H24A H 0.6326 0.8899 0.4087 0.073 Uiso 1 1 calc R . . C25 C 0.5156(7) 0.8370(7) 0.4498(5) 0.043(2) Uani 1 1 d . . . C26 C 0.4419(7) 0.9006(6) 0.4318(5) 0.042(2) Uani 1 1 d . . . C27 C 0.1996(7) 0.9422(6) 0.4400(5) 0.040(2) Uani 1 1 d . . . C28 C 0.1345(7) 0.8607(6) 0.4468(4) 0.034(2) Uani 1 1 d . . . C29 C 0.1487(7) 1.0257(6) 0.4337(6) 0.054(3) Uani 1 1 d . . . H29A H 0.1972 1.0738 0.4295 0.081 Uiso 1 1 calc R . . H29B H 0.1207 1.0447 0.4769 0.081 Uiso 1 1 calc R . . H29C H 0.0959 1.0117 0.3909 0.081 Uiso 1 1 calc R . . C30 C 0.0225(7) 0.8569(7) 0.4323(5) 0.051(3) Uani 1 1 d . . . H30A H -0.0074 0.8003 0.4400 0.076 Uiso 1 1 calc R . . H30B H -0.0007 0.8614 0.3824 0.076 Uiso 1 1 calc R . . H30C H 0.0036 0.9065 0.4654 0.076 Uiso 1 1 calc R . . C31 C 0.2613(17) 0.8019(13) 1.0344(10) 0.183(10) Uani 1 1 d . . . H31A H 0.2606 0.7753 1.0765 0.274 Uiso 1 1 calc R . . H31B H 0.2571 0.7548 0.9913 0.274 Uiso 1 1 calc R . . H31C H 0.2049 0.8353 1.0279 0.274 Uiso 1 1 calc R . . C32 C 0.6325(13) 0.0496(13) 0.2842(11) 0.124(6) Uani 1 1 d . . . C33 C 0.3203(16) 0.1387(12) 0.3117(11) 0.137(7) Uani 1 1 d . . . C34 C 0.727(2) -0.140(2) 0.2307(19) 0.135(15) Uani 0.50 1 d P . . N1 N 0.0626(5) 0.9252(5) 0.7832(4) 0.0338(17) Uani 1 1 d . . . N2 N 0.2747(6) 0.9947(5) 0.9322(4) 0.060(2) Uani 1 1 d . . . H2B H 0.2660 1.0488 0.9523 0.072 Uiso 1 1 calc R . . N3 N 0.2254(5) 0.8639(5) 0.8395(4) 0.0387(18) Uani 1 1 d . . . N4 N 0.3086(5) 0.8317(5) 0.8737(4) 0.0413(19) Uani 1 1 d . . . N5 N 0.2131(5) 0.7008(4) 0.7355(4) 0.0307(16) Uani 1 1 d . . . N6 N -0.0188(5) 0.4031(5) 0.8675(4) 0.0380(18) Uani 1 1 d . . . N7 N -0.2207(6) 0.4657(6) 0.9653(4) 0.053(2) Uani 1 1 d . . . H7A H -0.2096 0.4434 1.0040 0.064 Uiso 1 1 calc R . . N8 N -0.1756(5) 0.4900(5) 0.8556(4) 0.0394(18) Uani 1 1 d . . . N9 N -0.2600(6) 0.5359(5) 0.8498(4) 0.044(2) Uani 1 1 d . . . N10 N -0.1704(5) 0.5303(5) 0.7182(3) 0.0324(17) Uani 1 1 d . . . N11 N 0.4822(5) 0.7731(5) 0.4823(4) 0.0408(19) Uani 1 1 d . . . N12 N 0.4670(6) 0.9663(5) 0.3977(5) 0.061(2) Uani 1 1 d . . . H12B H 0.4246 1.0028 0.3872 0.073 Uiso 1 1 calc R . . H12C H 0.5256 0.9721 0.3863 0.073 Uiso 1 1 calc R . . N13 N 0.3551(5) 0.8863(5) 0.4514(4) 0.0370(18) Uani 1 1 d . . . N14 N 0.2947(6) 0.9542(5) 0.4398(4) 0.046(2) Uani 1 1 d . . . N15 N 0.1763(5) 0.7938(5) 0.4679(4) 0.0343(17) Uani 1 1 d . . . N16 N -0.0048(5) 0.6312(4) 0.5706(3) 0.0260(15) Uani 1 1 d . . . N17 N -0.0681(6) 0.6848(5) 0.5639(4) 0.045(2) Uani 1 1 d . . . N18 N -0.1175(8) 0.7388(7) 0.5611(6) 0.086(3) Uani 1 1 d . . . N19 N 0.1511(5) 0.5574(4) 0.5080(3) 0.0236(15) Uani 1 1 d . . . N20 N 0.2289(6) 0.5162(6) 0.5204(5) 0.054(2) Uani 1 1 d . . . N21 N 0.3056(11) 0.4958(9) 0.5325(9) 0.133(5) Uani 1 1 d . . . N22 N 0.0244(4) 0.4573(4) 0.6030(3) 0.0204(14) Uani 1 1 d . . . N23 N 0.0929(7) 0.4101(6) 0.6225(5) 0.053(2) Uani 1 1 d . . . N24 N 0.1474(12) 0.3713(11) 0.6444(10) 0.150(6) Uani 1 1 d . . . N25 N -0.0935(5) 0.3522(5) 0.6978(4) 0.0398(18) Uani 1 1 d . . . N26 N -0.1059(8) 0.2783(7) 0.7102(4) 0.063(3) Uani 1 1 d . . . N27 N -0.1166(14) 0.2084(7) 0.7231(6) 0.147(7) Uani 1 1 d . . . N28 N -0.0012(5) 0.7152(5) 0.7380(4) 0.0345(17) Uani 1 1 d . . . N29 N -0.0373(6) 0.7220(5) 0.7910(5) 0.049(2) Uani 1 1 d . . . N30 N -0.0738(9) 0.7277(7) 0.8415(6) 0.103(4) Uani 1 1 d . . . N31 N 0.1267(5) 0.8169(5) 0.6404(4) 0.0380(18) Uani 1 1 d . . . N32 N 0.1196(6) 0.8887(6) 0.6223(4) 0.0407(19) Uani 1 1 d . . . N33 N 0.1138(8) 0.9563(6) 0.6066(5) 0.067(3) Uani 1 1 d . . . N34 N 0.0485(6) 0.5352(5) 0.7728(4) 0.0384(18) Uani 1 1 d . . . N35 N 0.1094(6) 0.5675(5) 0.8274(4) 0.0419(19) Uani 1 1 d . . . N36 N 0.1698(7) 0.5967(7) 0.8800(5) 0.071(3) Uani 1 1 d . . . N37 N 0.3086(5) 0.7353(5) 0.5834(4) 0.0356(17) Uani 1 1 d . . . N38 N 0.3811(6) 0.7237(6) 0.6273(4) 0.047(2) Uani 1 1 d . . . N39 N 0.4478(7) 0.7147(8) 0.6681(5) 0.080(3) Uani 1 1 d . . . N40 N 0.5260(6) 0.9502(6) 0.9422(5) 0.065(3) Uani 1 1 d . . . N41 N 0.5495(7) 0.9131(7) 0.8863(5) 0.068(3) Uani 1 1 d . . . N42 N 0.5743(9) 0.8774(9) 0.8346(6) 0.108(4) Uani 1 1 d . . . N43 N 0.2854(5) 0.6474(5) 0.4135(4) 0.0394(18) Uani 1 1 d D . . N44 N 0.3487(10) 0.5993(9) 0.3957(8) 0.059(5) Uani 0.665(18) 1 d P A 1 N44' N 0.326(2) 0.6456(19) 0.3621(11) 0.059(5) Uani 0.34 1 d PD A 2 N45 N 0.4089(9) 0.5561(11) 0.3777(12) 0.139(10) Uani 0.665(18) 1 d PD A 1 N45' N 0.360(2) 0.644(2) 0.3079(11) 0.139(10) Uani 0.34 1 d PD A 2 N46 N -0.4692(9) 0.4669(10) 0.8940(7) 0.112(4) Uani 1 1 d . . . N47 N -0.5419(12) 0.4825(10) 0.9218(7) 0.114(4) Uani 1 1 d . . . N48 N -0.6248(11) 0.4856(12) 0.9408(8) 0.152(7) Uani 1 1 d . . . N49 N -0.3465(10) 0.6637(10) 0.9803(7) 0.108(4) Uani 1 1 d D . . N50 N -0.3056(16) 0.7348(14) 0.9772(12) 0.076(8) Uiso 0.478(16) 1 d PD B 1 N50' N -0.3534(19) 0.7221(15) 1.0305(11) 0.116(10) Uiso 0.522(16) 1 d PD B 2 N51 N -0.2601(16) 0.8022(12) 0.9692(11) 0.079(8) Uiso 0.478(16) 1 d PD B 1 N51' N -0.376(3) 0.767(2) 1.0838(14) 0.200(17) Uiso 0.522(16) 1 d PD B 2 O1 O 0.1721(4) 0.6345(4) 0.6723(3) 0.0325(14) Uani 1 1 d . . . O2 O -0.1347(4) 0.5320(4) 0.6538(3) 0.0344(14) Uani 1 1 d . . . O3 O 0.1113(4) 0.7207(4) 0.4749(3) 0.0330(14) Uani 1 1 d . . . O4 O 0.3593(8) 0.8666(6) 1.0464(4) 0.097(3) Uani 1 1 d . . . O5 O 0.6014(12) -0.0353(11) 0.2912(11) 0.075(7) Uani 0.64(4) 1 d P . . O5' O 0.649(3) 0.015(3) 0.351(3) 0.119(18) Uani 0.36(4) 1 d P . . O6 O 0.3374(12) 0.0576(11) 0.2977(8) 0.189(7) Uani 1 1 d . . . O7 O 0.4003(16) 0.9071(13) 0.1926(8) 0.118(8) Uani 0.50 1 d P . . O8 O 0.578(3) 0.647(3) 0.259(2) 0.29(2) Uani 0.50 1 d P . . O10 O 0.798(2) -0.1687(15) 0.2723(16) 0.184(13) Uani 0.50 1 d P . . O9 O 0.391(2) 0.757(2) 0.2489(14) 0.212(16) Uani 0.50 1 d P C 1 C36 C -0.160(3) 0.918(2) 0.9164(14) 0.138(14) Uani 0.50 1 d P D 2 O11 O -0.2040(16) 0.8470(14) 0.9578(11) 0.109(6) Uiso 0.50 1 d P D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0311(8) 0.0331(8) 0.0269(7) 0.0059(6) 0.0030(6) 0.0044(6) Zn2 0.0349(6) 0.0344(6) 0.0284(5) 0.0060(5) 0.0059(4) 0.0049(5) Zn3 0.0342(6) 0.0337(6) 0.0258(5) 0.0058(4) 0.0042(4) 0.0039(5) Zn4 0.0352(6) 0.0337(6) 0.0273(5) 0.0070(4) 0.0036(4) 0.0042(5) Zn5 0.0404(6) 0.0393(6) 0.0269(5) 0.0095(5) 0.0092(5) 0.0096(5) Zn6 0.0361(6) 0.0332(6) 0.0296(5) 0.0038(4) 0.0019(4) 0.0078(5) Zn7 0.0337(6) 0.0365(6) 0.0401(6) 0.0116(5) 0.0063(5) 0.0046(5) Zn8 0.0481(7) 0.0558(8) 0.0452(7) -0.0008(6) -0.0024(6) 0.0032(6) Zn9 0.0742(10) 0.0873(11) 0.0760(10) 0.0148(8) 0.0270(8) 0.0204(8) C1 0.063(7) 0.038(6) 0.041(6) 0.004(5) 0.002(5) 0.013(5) C2 0.068(8) 0.064(8) 0.075(8) 0.009(7) -0.005(6) 0.034(7) C3 0.088(10) 0.060(8) 0.108(11) -0.016(8) -0.011(8) 0.038(7) C4 0.086(9) 0.063(8) 0.078(9) -0.023(7) -0.026(7) 0.033(7) C5 0.043(6) 0.037(6) 0.050(6) 0.003(5) 0.000(5) 0.011(5) C6 0.047(6) 0.032(5) 0.041(6) 0.000(5) 0.000(5) 0.000(5) C7 0.032(5) 0.053(6) 0.040(6) 0.011(5) -0.002(4) 0.009(5) C8 0.026(5) 0.033(5) 0.032(5) 0.004(4) 0.004(4) 0.002(4) C9 0.058(7) 0.051(6) 0.049(6) 0.000(5) -0.015(5) 0.011(5) C10 0.039(6) 0.049(6) 0.042(5) 0.011(5) -0.002(4) 0.015(5) C11 0.059(7) 0.056(6) 0.035(6) 0.011(5) 0.011(5) 0.016(6) C12 0.068(7) 0.056(7) 0.041(6) 0.010(5) 0.005(5) 0.024(6) C13 0.082(9) 0.063(7) 0.043(6) 0.028(6) -0.008(6) 0.007(7) C14 0.064(7) 0.051(6) 0.036(6) 0.020(5) 0.011(5) 0.003(6) C15 0.055(6) 0.035(5) 0.033(5) 0.002(4) 0.000(5) -0.005(5) C16 0.040(6) 0.040(6) 0.037(5) 0.009(5) 0.002(4) -0.002(5) C17 0.041(6) 0.064(7) 0.041(6) 0.018(5) 0.015(5) 0.024(5) C18 0.038(6) 0.053(6) 0.044(6) 0.012(5) 0.006(5) 0.021(5) C19 0.063(8) 0.099(9) 0.078(8) 0.035(7) 0.035(6) 0.041(7) C20 0.092(10) 0.139(12) 0.076(8) 0.052(8) 0.036(7) 0.082(9) C21 0.042(6) 0.065(7) 0.059(7) 0.018(6) 0.005(5) 0.016(6) C22 0.043(7) 0.075(8) 0.090(9) 0.023(7) 0.011(6) 0.018(6) C23 0.040(7) 0.096(10) 0.098(10) 0.029(8) 0.013(6) 0.010(7) C24 0.048(7) 0.058(7) 0.084(8) 0.025(6) 0.017(6) 0.016(6) C25 0.034(6) 0.050(6) 0.044(6) 0.009(5) 0.007(4) 0.003(5) C26 0.042(6) 0.041(6) 0.046(6) 0.014(5) 0.012(5) 0.002(5) C27 0.048(6) 0.040(6) 0.039(5) 0.014(4) 0.015(5) 0.010(5) C28 0.048(6) 0.031(5) 0.023(5) 0.001(4) 0.005(4) 0.006(5) C29 0.051(7) 0.037(6) 0.083(8) 0.026(5) 0.019(6) 0.013(5) C30 0.041(6) 0.051(6) 0.059(6) 0.013(5) -0.002(5) 0.016(5) C31 0.27(3) 0.130(16) 0.125(16) 0.047(13) -0.002(17) -0.057(18) C32 0.113(14) 0.126(16) 0.133(16) 0.051(12) 0.011(11) -0.018(11) C33 0.19(2) 0.094(12) 0.152(16) 0.034(12) 0.089(15) 0.025(13) C34 0.10(2) 0.14(3) 0.13(3) -0.05(2) -0.026(19) 0.08(2) N1 0.034(4) 0.033(4) 0.033(4) 0.005(3) 0.001(3) 0.010(4) N2 0.063(6) 0.047(5) 0.054(5) -0.014(4) -0.015(5) 0.016(5) N3 0.034(4) 0.041(5) 0.033(4) -0.001(4) -0.006(3) 0.007(4) N4 0.034(4) 0.040(5) 0.043(5) -0.001(4) 0.001(4) 0.008(4) N5 0.027(4) 0.034(4) 0.031(4) 0.008(3) 0.004(3) 0.003(3) N6 0.041(5) 0.040(4) 0.034(4) 0.005(4) 0.011(4) 0.008(4) N7 0.065(6) 0.073(6) 0.031(4) 0.020(4) 0.023(4) 0.009(5) N8 0.045(5) 0.041(5) 0.034(4) 0.008(4) 0.013(4) 0.003(4) N9 0.040(5) 0.049(5) 0.045(5) 0.002(4) 0.019(4) 0.011(4) N10 0.035(4) 0.040(4) 0.024(4) 0.007(3) 0.009(3) 0.005(4) N11 0.034(5) 0.044(5) 0.041(4) 0.011(4) 0.000(4) -0.003(4) N12 0.053(6) 0.053(6) 0.090(7) 0.027(5) 0.032(5) 0.014(5) N13 0.032(4) 0.038(4) 0.044(4) 0.014(4) 0.009(4) 0.010(4) N14 0.050(5) 0.042(5) 0.055(5) 0.019(4) 0.019(4) 0.014(4) N15 0.032(4) 0.038(4) 0.032(4) 0.009(3) 0.005(3) 0.005(4) N16 0.028(4) 0.031(4) 0.022(4) 0.010(3) 0.007(3) 0.009(3) N17 0.048(5) 0.040(5) 0.050(5) 0.010(4) 0.015(4) 0.020(4) N18 0.084(8) 0.080(8) 0.093(8) 0.014(6) 0.016(6) 0.020(7) N19 0.019(4) 0.029(4) 0.022(3) 0.006(3) -0.001(3) 0.004(3) N20 0.035(5) 0.072(6) 0.057(6) 0.017(5) 0.007(4) 0.020(5) N21 0.115(12) 0.115(11) 0.166(14) 0.024(10) 0.020(10) 0.020(10) N22 0.022(4) 0.024(4) 0.014(3) 0.004(3) -0.003(3) 0.009(3) N23 0.057(6) 0.050(6) 0.056(6) 0.020(5) 0.007(5) 0.016(5) N24 0.132(14) 0.136(14) 0.199(17) 0.061(12) 0.033(12) 0.040(11) N25 0.044(5) 0.043(5) 0.033(4) 0.008(4) 0.007(3) 0.007(4) N26 0.117(9) 0.044(6) 0.033(5) 0.013(4) 0.013(5) 0.028(6) N27 0.34(2) 0.045(7) 0.057(7) 0.020(6) 0.023(10) 0.036(10) N28 0.041(4) 0.034(4) 0.026(4) 0.005(3) 0.003(3) 0.003(4) N29 0.058(6) 0.045(5) 0.039(5) -0.003(4) 0.015(4) 0.000(4) N30 0.148(11) 0.085(8) 0.066(7) -0.021(6) 0.059(7) -0.023(7) N31 0.040(5) 0.042(5) 0.029(4) 0.006(4) -0.001(3) 0.009(4) N32 0.053(5) 0.042(5) 0.027(4) 0.004(4) 0.006(4) 0.017(4) N33 0.108(8) 0.051(6) 0.057(6) 0.027(5) 0.028(5) 0.031(6) N34 0.040(5) 0.045(5) 0.029(4) 0.009(4) 0.002(4) 0.005(4) N35 0.037(5) 0.053(5) 0.037(5) 0.014(4) 0.009(4) 0.001(4) N36 0.060(6) 0.111(8) 0.039(5) 0.026(5) 0.007(5) -0.016(6) N37 0.032(4) 0.043(5) 0.032(4) 0.010(4) 0.005(3) 0.002(4) N38 0.035(5) 0.066(6) 0.040(5) 0.020(4) 0.003(4) -0.002(4) N39 0.045(6) 0.137(10) 0.070(7) 0.058(7) -0.001(5) 0.010(6) N40 0.049(5) 0.076(6) 0.051(5) -0.020(5) 0.000(4) -0.002(5) N41 0.072(7) 0.081(7) 0.045(6) 0.001(5) 0.013(5) -0.002(5) N42 0.122(10) 0.125(10) 0.064(7) -0.012(7) 0.029(7) -0.006(8) N43 0.038(5) 0.042(5) 0.038(4) 0.003(4) 0.013(4) 0.005(4) N44 0.047(8) 0.052(10) 0.068(11) -0.015(7) 0.014(7) 0.007(7) N44' 0.047(8) 0.052(10) 0.068(11) -0.015(7) 0.014(7) 0.007(7) N45 0.036(9) 0.100(13) 0.22(2) -0.087(13) 0.016(10) -0.001(8) N45' 0.036(9) 0.100(13) 0.22(2) -0.087(13) 0.016(10) -0.001(8) N46 0.056(7) 0.162(13) 0.118(10) 0.027(9) 0.028(7) -0.001(8) N47 0.116(12) 0.139(12) 0.096(9) 0.045(9) 0.019(9) 0.024(10) N48 0.107(11) 0.252(19) 0.144(13) 0.076(12) 0.086(10) 0.085(12) N49 0.109(10) 0.126(11) 0.082(8) -0.003(8) -0.001(7) 0.064(9) O1 0.032(3) 0.033(3) 0.026(3) -0.002(3) 0.001(3) -0.002(3) O2 0.038(3) 0.038(3) 0.025(3) 0.002(3) 0.005(3) 0.004(3) O3 0.035(3) 0.033(3) 0.032(3) 0.009(3) 0.005(3) 0.003(3) O4 0.134(8) 0.086(6) 0.061(5) 0.020(5) 0.000(5) -0.012(6) O5 0.081(11) 0.055(10) 0.097(15) 0.018(9) 0.038(10) 0.004(8) O5' 0.08(2) 0.15(3) 0.14(4) 0.02(3) 0.05(2) 0.00(2) O6 0.279(18) 0.203(15) 0.178(13) 0.123(12) 0.137(13) 0.155(14) O7 0.163(19) 0.111(15) 0.042(9) 0.017(9) -0.040(10) -0.071(14) O8 0.24(4) 0.29(4) 0.29(4) -0.12(3) 0.17(3) -0.06(3) O10 0.20(3) 0.092(17) 0.23(3) 0.064(17) -0.09(2) 0.025(17) O9 0.28(4) 0.32(4) 0.14(2) 0.13(2) 0.13(2) 0.23(3) C36 0.23(4) 0.17(3) 0.049(16) 0.040(19) 0.08(2) 0.09(3) _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 N19 2.122(6) 2_566 ? Zn1 N19 2.122(6) . ? Zn1 N22 2.150(6) . ? Zn1 N22 2.150(6) 2_566 ? Zn1 N16 2.173(6) 2_566 ? Zn1 N16 2.173(6) . ? Zn2 O3 2.091(5) 2_566 ? Zn2 O2 2.105(5) . ? Zn2 N43 2.127(7) 2_566 ? Zn2 N25 2.160(8) . ? Zn2 N22 2.172(6) . ? Zn2 N19 2.186(6) 2_566 ? Zn3 O2 2.124(6) . ? Zn3 O1 2.137(5) . ? Zn3 N28 2.149(7) . ? Zn3 N22 2.151(6) . ? Zn3 N34 2.153(7) . ? Zn3 N16 2.167(6) . ? Zn4 O3 2.087(5) . ? Zn4 O1 2.097(5) . ? Zn4 N37 2.144(7) . ? Zn4 N31 2.149(7) . ? Zn4 N19 2.155(6) . ? Zn4 N16 2.209(6) . ? Zn5 N8 2.026(7) . ? Zn5 N25 2.043(7) . ? Zn5 N10 2.052(7) . ? Zn5 N34 2.068(8) . ? Zn5 N6 2.084(7) . ? Zn6 N3 2.023(7) . ? Zn6 N31 2.037(7) . ? Zn6 N28 2.058(7) . ? Zn6 N5 2.071(6) . ? Zn6 N1 2.113(6) . ? Zn7 N13 2.031(7) . ? Zn7 N43 2.035(7) . ? Zn7 N37 2.042(7) . ? Zn7 N15 2.073(7) . ? Zn7 N11 2.144(7) . ? Zn8 N2 1.952(8) . ? Zn8 N40 2.020(9) . ? Zn8 O4 2.021(9) . ? Zn8 N40 2.160(8) 2_677 ? Zn8 N4 2.257(7) . ? Zn9 N49 1.955(13) . ? Zn9 N7 1.986(8) . ? Zn9 N46 1.989(12) . ? Zn9 N9 2.231(7) . ? Zn9 N48 2.360(13) 2_467 ? C1 N1 1.335(11) . ? C1 C2 1.377(13) . ? C2 C3 1.406(15) . ? C3 C4 1.375(15) . ? C4 C5 1.363(13) . ? C5 N1 1.315(11) . ? C5 C6 1.493(12) . ? C6 N2 1.294(11) . ? C6 N3 1.359(10) . ? C7 N4 1.286(11) . ? C7 C8 1.491(12) . ? C7 C9 1.520(12) . ? C8 N5 1.273(10) . ? C8 C10 1.495(11) . ? C11 N6 1.342(11) . ? C11 C12 1.374(13) . ? C12 C13 1.388(14) . ? C13 C14 1.372(14) . ? C14 C15 1.401(13) . ? C15 N6 1.370(11) . ? C15 C16 1.496(13) . ? C16 N8 1.330(11) . ? C16 N7 1.331(11) . ? C17 N9 1.289(11) . ? C17 C18 1.493(12) . ? C17 C19 1.503(12) . ? C18 N10 1.266(10) . ? C18 C20 1.476(14) . ? C21 N11 1.328(11) . ? C21 C22 1.347(13) . ? C22 C23 1.380(16) . ? C23 C24 1.379(15) . ? C24 C25 1.396(13) . ? C25 N11 1.326(11) . ? C25 C26 1.495(13) . ? C26 N13 1.307(11) . ? C26 N12 1.334(11) . ? C27 N14 1.288(11) . ? C27 C28 1.488(12) . ? C27 C29 1.511(12) . ? C28 N15 1.302(10) . ? C28 C30 1.494(12) . ? C31 O4 1.53(2) . ? C32 O5 1.35(2) . ? C32 O5' 1.44(4) . ? C33 O6 1.254(18) . ? C34 O10 1.30(3) . ? N3 N4 1.383(9) . ? N5 O1 1.392(8) . ? N8 N9 1.394(10) . ? N10 O2 1.384(8) . ? N13 N14 1.400(10) . ? N15 O3 1.390(9) . ? N16 N17 1.244(9) . ? N17 N18 1.107(11) . ? N19 N20 1.288(10) . ? N19 Zn2 2.186(6) 2_566 ? N20 N21 1.114(14) . ? N22 N23 1.275(10) . ? N23 N24 1.065(15) . ? N25 N26 1.188(11) . ? N26 N27 1.132(13) . ? N28 N29 1.177(10) . ? N29 N30 1.138(11) . ? N31 N32 1.208(10) . ? N32 N33 1.125(11) . ? N34 N35 1.193(10) . ? N35 N36 1.157(11) . ? N37 N38 1.226(10) . ? N38 N39 1.124(11) . ? N40 N41 1.201(11) . ? N40 Zn8 2.160(8) 2_677 ? N41 N42 1.136(12) . ? N43 N44' 1.191(8) . ? N43 N44 1.224(13) . ? N43 Zn2 2.127(7) 2_566 ? N44 N45 1.149(14) . ? N44' N45' 1.189(9) . ? N46 N47 1.216(16) . ? N47 N48 1.239(16) . ? N48 Zn9 2.360(13) 2_467 ? N49 N50 1.180(8) . ? N49 N50' 1.183(9) . ? N50 N51 1.191(8) . ? N50' N51' 1.201(9) . ? O3 Zn2 2.091(5) 2_566 ? O5 O5' 1.26(4) . ? C36 O11 1.58(4) . ? 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 N19 Zn1 N19 180.0(3) 2_566 . ? N19 Zn1 N22 83.9(2) 2_566 . ? N19 Zn1 N22 96.1(2) . . ? N19 Zn1 N22 96.1(2) 2_566 2_566 ? N19 Zn1 N22 83.9(2) . 2_566 ? N22 Zn1 N22 180.000(1) . 2_566 ? N19 Zn1 N16 81.6(2) 2_566 2_566 ? N19 Zn1 N16 98.4(2) . 2_566 ? N22 Zn1 N16 97.1(2) . 2_566 ? N22 Zn1 N16 82.9(2) 2_566 2_566 ? N19 Zn1 N16 98.4(2) 2_566 . ? N19 Zn1 N16 81.6(2) . . ? N22 Zn1 N16 82.9(2) . . ? N22 Zn1 N16 97.1(2) 2_566 . ? N16 Zn1 N16 180.000(1) 2_566 . ? O3 Zn2 O2 168.3(2) 2_566 . ? O3 Zn2 N43 91.1(2) 2_566 2_566 ? O2 Zn2 N43 96.0(2) . 2_566 ? O3 Zn2 N25 97.1(2) 2_566 . ? O2 Zn2 N25 92.0(2) . . ? N43 Zn2 N25 91.2(3) 2_566 . ? O3 Zn2 N22 92.0(2) 2_566 . ? O2 Zn2 N22 80.2(2) . . ? N43 Zn2 N22 174.4(3) 2_566 . ? N25 Zn2 N22 93.1(3) . . ? O3 Zn2 N19 79.8(2) 2_566 2_566 ? O2 Zn2 N19 90.5(2) . 2_566 ? N43 Zn2 N19 94.0(3) 2_566 2_566 ? N25 Zn2 N19 174.0(2) . 2_566 ? N22 Zn2 N19 81.9(2) . 2_566 ? O2 Zn3 O1 169.45(19) . . ? O2 Zn3 N28 94.5(2) . . ? O1 Zn3 N28 91.9(2) . . ? O2 Zn3 N22 80.3(2) . . ? O1 Zn3 N22 92.8(2) . . ? N28 Zn3 N22 173.9(2) . . ? O2 Zn3 N34 90.9(3) . . ? O1 Zn3 N34 97.5(2) . . ? N28 Zn3 N34 89.6(3) . . ? N22 Zn3 N34 93.6(2) . . ? O2 Zn3 N16 90.0(2) . . ? O1 Zn3 N16 81.2(2) . . ? N28 Zn3 N16 93.9(3) . . ? N22 Zn3 N16 83.0(2) . . ? N34 Zn3 N16 176.3(2) . . ? O3 Zn4 O1 168.3(2) . . ? O3 Zn4 N37 92.2(2) . . ? O1 Zn4 N37 97.1(2) . . ? O3 Zn4 N31 95.5(2) . . ? O1 Zn4 N31 91.1(2) . . ? N37 Zn4 N31 93.2(3) . . ? O3 Zn4 N19 80.6(2) . . ? O1 Zn4 N19 91.3(2) . . ? N37 Zn4 N19 96.1(2) . . ? N31 Zn4 N19 170.0(3) . . ? O3 Zn4 N16 89.1(2) . . ? O1 Zn4 N16 81.1(2) . . ? N37 Zn4 N16 175.7(2) . . ? N31 Zn4 N16 90.7(3) . . ? N19 Zn4 N16 80.1(2) . . ? N8 Zn5 N25 129.6(3) . . ? N8 Zn5 N10 86.3(3) . . ? N25 Zn5 N10 92.5(3) . . ? N8 Zn5 N34 130.4(3) . . ? N25 Zn5 N34 100.0(3) . . ? N10 Zn5 N34 92.3(3) . . ? N8 Zn5 N6 78.8(3) . . ? N25 Zn5 N6 97.7(3) . . ? N10 Zn5 N6 165.0(3) . . ? N34 Zn5 N6 96.7(3) . . ? N3 Zn6 N31 129.5(3) . . ? N3 Zn6 N28 126.1(3) . . ? N31 Zn6 N28 104.4(3) . . ? N3 Zn6 N5 86.5(3) . . ? N31 Zn6 N5 91.0(3) . . ? N28 Zn6 N5 91.1(3) . . ? N3 Zn6 N1 78.6(3) . . ? N31 Zn6 N1 99.3(3) . . ? N28 Zn6 N1 96.8(3) . . ? N5 Zn6 N1 165.0(3) . . ? N13 Zn7 N43 121.3(3) . . ? N13 Zn7 N37 136.4(3) . . ? N43 Zn7 N37 101.9(3) . . ? N13 Zn7 N15 85.4(3) . . ? N43 Zn7 N15 89.6(3) . . ? N37 Zn7 N15 90.2(3) . . ? N13 Zn7 N11 77.6(3) . . ? N43 Zn7 N11 94.1(3) . . ? N37 Zn7 N11 106.2(3) . . ? N15 Zn7 N11 162.0(3) . . ? N2 Zn8 N40 125.0(4) . . ? N2 Zn8 O4 112.7(4) . . ? N40 Zn8 O4 122.3(4) . . ? N2 Zn8 N40 102.4(3) . 2_677 ? N40 Zn8 N40 78.1(4) . 2_677 ? O4 Zn8 N40 91.6(4) . 2_677 ? N2 Zn8 N4 76.3(3) . . ? N40 Zn8 N4 97.9(3) . . ? O4 Zn8 N4 94.3(3) . . ? N40 Zn8 N4 174.0(3) 2_677 . ? N49 Zn9 N7 130.0(4) . . ? N49 Zn9 N46 110.7(6) . . ? N7 Zn9 N46 118.9(5) . . ? N49 Zn9 N9 102.5(5) . . ? N7 Zn9 N9 76.0(3) . . ? N46 Zn9 N9 99.9(4) . . ? N49 Zn9 N48 86.4(6) . 2_467 ? N7 Zn9 N48 87.6(4) . 2_467 ? N46 Zn9 N48 89.6(6) . 2_467 ? N9 Zn9 N48 163.5(4) . 2_467 ? N1 C1 C2 122.4(9) . . ? C1 C2 C3 116.7(10) . . ? C4 C3 C2 119.2(10) . . ? C5 C4 C3 120.1(10) . . ? N1 C5 C4 120.8(9) . . ? N1 C5 C6 115.9(7) . . ? C4 C5 C6 123.2(9) . . ? N2 C6 N3 122.5(8) . . ? N2 C6 C5 123.6(8) . . ? N3 C6 C5 113.9(8) . . ? N4 C7 C8 130.6(8) . . ? N4 C7 C9 115.0(8) . . ? C8 C7 C9 114.4(8) . . ? N5 C8 C7 119.5(7) . . ? N5 C8 C10 120.5(7) . . ? C7 C8 C10 119.9(7) . . ? N6 C11 C12 124.1(9) . . ? C11 C12 C13 116.9(9) . . ? C14 C13 C12 121.7(9) . . ? C13 C14 C15 118.0(9) . . ? N6 C15 C14 121.3(9) . . ? N6 C15 C16 114.2(8) . . ? C14 C15 C16 124.5(9) . . ? N8 C16 N7 123.2(8) . . ? N8 C16 C15 114.3(8) . . ? N7 C16 C15 122.4(8) . . ? N9 C17 C18 129.0(8) . . ? N9 C17 C19 116.1(8) . . ? C18 C17 C19 114.9(8) . . ? N10 C18 C20 120.2(8) . . ? N10 C18 C17 119.6(8) . . ? C20 C18 C17 120.2(8) . . ? N11 C21 C22 123.6(11) . . ? C21 C22 C23 118.4(11) . . ? C24 C23 C22 120.4(11) . . ? C23 C24 C25 116.1(11) . . ? N11 C25 C24 123.7(9) . . ? N11 C25 C26 114.9(8) . . ? C24 C25 C26 121.5(9) . . ? N13 C26 N12 124.5(9) . . ? N13 C26 C25 115.6(8) . . ? N12 C26 C25 119.9(8) . . ? N14 C27 C28 130.3(8) . . ? N14 C27 C29 113.4(8) . . ? C28 C27 C29 116.3(8) . . ? N15 C28 C27 119.2(8) . . ? N15 C28 C30 120.2(8) . . ? C27 C28 C30 120.6(8) . . ? O5 C32 O5' 53.4(17) . . ? C5 N1 C1 120.7(7) . . ? C5 N1 Zn6 114.4(6) . . ? C1 N1 Zn6 124.9(6) . . ? C6 N2 Zn8 118.5(6) . . ? C6 N3 N4 113.4(7) . . ? C6 N3 Zn6 116.8(6) . . ? N4 N3 Zn6 129.8(5) . . ? C7 N4 N3 121.7(7) . . ? C7 N4 Zn8 129.0(6) . . ? N3 N4 Zn8 109.2(5) . . ? C8 N5 O1 118.0(6) . . ? C8 N5 Zn6 131.2(5) . . ? O1 N5 Zn6 110.3(4) . . ? C11 N6 C15 118.1(8) . . ? C11 N6 Zn5 127.4(6) . . ? C15 N6 Zn5 114.5(6) . . ? C16 N7 Zn9 116.8(6) . . ? C16 N8 N9 112.8(7) . . ? C16 N8 Zn5 117.9(6) . . ? N9 N8 Zn5 129.1(6) . . ? C17 N9 N8 122.8(7) . . ? C17 N9 Zn9 126.0(6) . . ? N8 N9 Zn9 111.2(6) . . ? C18 N10 O2 116.6(7) . . ? C18 N10 Zn5 132.5(6) . . ? O2 N10 Zn5 110.5(4) . . ? C25 N11 C21 117.8(8) . . ? C25 N11 Zn7 113.2(6) . . ? C21 N11 Zn7 128.5(7) . . ? C26 N13 N14 112.1(7) . . ? C26 N13 Zn7 117.2(6) . . ? N14 N13 Zn7 130.6(5) . . ? C27 N14 N13 120.9(8) . . ? C28 N15 O3 116.3(7) . . ? C28 N15 Zn7 131.8(6) . . ? O3 N15 Zn7 111.8(5) . . ? N17 N16 Zn3 116.4(5) . . ? N17 N16 Zn1 128.6(6) . . ? Zn3 N16 Zn1 96.4(3) . . ? N17 N16 Zn4 115.3(5) . . ? Zn3 N16 Zn4 96.5(2) . . ? Zn1 N16 Zn4 97.5(2) . . ? N18 N17 N16 173.6(11) . . ? N20 N19 Zn1 125.1(6) . . ? N20 N19 Zn4 117.2(5) . . ? Zn1 N19 Zn4 100.8(2) . . ? N20 N19 Zn2 114.6(5) . 2_566 ? Zn1 N19 Zn2 97.3(2) . 2_566 ? Zn4 N19 Zn2 96.7(2) . 2_566 ? N21 N20 N19 167.3(13) . . ? N23 N22 Zn1 124.7(5) . . ? N23 N22 Zn3 118.3(5) . . ? Zn1 N22 Zn3 97.6(2) . . ? N23 N22 Zn2 116.4(6) . . ? Zn1 N22 Zn2 96.9(2) . . ? Zn3 N22 Zn2 97.8(2) . . ? N24 N23 N22 173.8(14) . . ? N26 N25 Zn5 118.2(6) . . ? N26 N25 Zn2 130.8(6) . . ? Zn5 N25 Zn2 107.4(4) . . ? N27 N26 N25 178.8(14) . . ? N29 N28 Zn6 115.8(6) . . ? N29 N28 Zn3 123.1(6) . . ? Zn6 N28 Zn3 107.8(3) . . ? N30 N29 N28 178.8(11) . . ? N32 N31 Zn6 121.0(6) . . ? N32 N31 Zn4 129.6(6) . . ? Zn6 N31 Zn4 109.2(4) . . ? N33 N32 N31 178.8(10) . . ? N35 N34 Zn5 118.3(6) . . ? N35 N34 Zn3 127.4(6) . . ? Zn5 N34 Zn3 108.4(3) . . ? N36 N35 N34 178.1(11) . . ? N38 N37 Zn7 121.5(6) . . ? N38 N37 Zn4 127.5(6) . . ? Zn7 N37 Zn4 108.8(3) . . ? N39 N38 N37 178.8(11) . . ? N41 N40 Zn8 128.5(7) . . ? N41 N40 Zn8 128.9(7) . 2_677 ? Zn8 N40 Zn8 101.9(4) . 2_677 ? N42 N41 N40 178.0(13) . . ? N44' N43 N44 52.3(13) . . ? N44' N43 Zn7 110.6(14) . . ? N44 N43 Zn7 121.3(8) . . ? N44' N43 Zn2 123.4(15) . 2_566 ? N44 N43 Zn2 125.2(8) . 2_566 ? Zn7 N43 Zn2 110.6(3) . 2_566 ? N45 N44 N43 178(2) . . ? N45' N44' N43 175(3) . . ? N47 N46 Zn9 117.9(12) . . ? N46 N47 N48 168.9(18) . . ? N47 N48 Zn9 127.0(12) . 2_467 ? N50 N49 N50' 68.0(17) . . ? N50 N49 Zn9 137.8(16) . . ? N50' N49 Zn9 146.7(17) . . ? N49 N50 N51 174(3) . . ? N49 N50' N51' 166(3) . . ? N5 O1 Zn4 111.8(4) . . ? N5 O1 Zn3 110.4(4) . . ? Zn4 O1 Zn3 100.9(2) . . ? N10 O2 Zn2 110.2(4) . . ? N10 O2 Zn3 112.7(4) . . ? Zn2 O2 Zn3 100.8(2) . . ? N15 O3 Zn4 110.4(4) . . ? N15 O3 Zn2 110.5(4) . 2_566 ? Zn4 O3 Zn2 101.8(2) . 2_566 ? C31 O4 Zn8 122.4(9) . . ? O5' O5 C32 66.9(19) . . ? O5 O5' C32 60(2) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 23.37 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.874 _refine_diff_density_min -1.290 _refine_diff_density_rms 0.120 data_1 _database_code_depnum_ccdc_archive 'CCDC 656073' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H13 N14 Zn2' _chemical_formula_weight 496.11 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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6683(2) _cell_length_b 10.2683(2) _cell_length_c 18.9476(7) _cell_angle_alpha 90.00 _cell_angle_beta 117.949(3) _cell_angle_gamma 90.00 _cell_volume 1833.53(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 39057 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour 'Light yellow' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 2.651 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.510 _exptl_absorpt_correction_T_max 0.790 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31994 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4168 _reflns_number_gt 2744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0696P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4168 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1266 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 0.00486(4) 0.83871(4) 0.39909(3) 0.04061(17) Uani 1 1 d . . . Zn2 Zn -0.35421(5) 1.01360(5) 0.48428(3) 0.04301(17) Uani 1 1 d . . . C1 C 0.2206(4) 0.6305(4) 0.5095(3) 0.0549(12) Uani 1 1 d . . . H1A H 0.2634 0.6417 0.4770 0.066 Uiso 1 1 calc R . . C2 C 0.2742(5) 0.5382(5) 0.5689(3) 0.0633(13) Uani 1 1 d . . . H2A H 0.3528 0.4890 0.5766 0.076 Uiso 1 1 calc R . . C3 C 0.2120(5) 0.5194(5) 0.6159(3) 0.0648(14) Uani 1 1 d . . . H3A H 0.2476 0.4571 0.6562 0.078 Uiso 1 1 calc R . . C4 C 0.0938(5) 0.5942(4) 0.6037(3) 0.0524(11) Uani 1 1 d . . . H4A H 0.0488 0.5818 0.6350 0.063 Uiso 1 1 calc R . . C5 C 0.0456(4) 0.6874(4) 0.5437(2) 0.0382(9) Uani 1 1 d . . . C6 C -0.0761(4) 0.7731(4) 0.5274(2) 0.0387(9) Uani 1 1 d . . . C7 C -0.2273(4) 1.0044(4) 0.3779(2) 0.0372(9) Uani 1 1 d . . . C8 C -0.3467(4) 1.0982(4) 0.3403(2) 0.0371(8) Uani 1 1 d . . . C9 C -0.3796(5) 1.1618(4) 0.2688(3) 0.0555(11) Uani 1 1 d . . . H9A H -0.3248 1.1501 0.2430 0.067 Uiso 1 1 calc R . . C10 C -0.4980(5) 1.2437(5) 0.2374(3) 0.0673(14) Uani 1 1 d . . . H10A H -0.5217 1.2892 0.1904 0.081 Uiso 1 1 calc R . . C11 C -0.5784(5) 1.2571(5) 0.2749(3) 0.0613(13) Uani 1 1 d . . . H11A H -0.6590 1.3094 0.2531 0.074 Uiso 1 1 calc R . . C12 C -0.5393(4) 1.1926(4) 0.3454(3) 0.0532(11) Uani 1 1 d . . . H12A H -0.5942 1.2032 0.3713 0.064 Uiso 1 1 calc R . . C13 C -0.1456(5) 0.7611(5) 0.5796(3) 0.0582(12) Uani 1 1 d . . . H13A H -0.2227 0.8219 0.5624 0.087 Uiso 1 1 calc R . . H13B H -0.0776 0.7794 0.6339 0.087 Uiso 1 1 calc R . . H13C H -0.1813 0.6742 0.5760 0.087 Uiso 1 1 calc R . . N1 N 0.1084(3) 0.7052(3) 0.4967(2) 0.0422(8) Uani 1 1 d . . . N2 N -0.1099(3) 0.8487(3) 0.46743(19) 0.0403(8) Uani 1 1 d . . . N3 N -0.2210(3) 0.9374(3) 0.44087(19) 0.0381(7) Uani 1 1 d . . . N4 N -0.4247(3) 1.1144(3) 0.37886(19) 0.0393(7) Uani 1 1 d . . . N5 N -0.1347(4) 0.9875(3) 0.3503(2) 0.0457(8) Uani 1 1 d . . . N6 N -0.0554(4) 0.7130(4) 0.3079(2) 0.0624(11) Uani 1 1 d . . . N7 N 0.0248(5) 0.6414(4) 0.3003(2) 0.0640(11) Uani 1 1 d . . . N8 N 0.1004(7) 0.5707(6) 0.2919(4) 0.110(2) Uani 1 1 d . . . N9 N 0.1966(3) 0.9148(3) 0.4126(2) 0.0420(8) Uani 1 1 d . . . N10 N 0.2166(4) 0.9139(4) 0.3547(2) 0.0488(9) Uani 1 1 d . . . N11 N 0.2356(5) 0.9150(6) 0.3013(3) 0.0865(15) Uani 1 1 d . . . N12 N -0.4853(3) 0.8763(4) 0.4853(2) 0.0473(9) Uani 1 1 d . . . N13 N -0.5028(4) 0.7665(4) 0.4584(2) 0.0552(10) Uani 1 1 d . . . N14 N -0.5256(5) 0.6632(5) 0.4347(4) 0.0932(17) Uani 1 1 d . . . 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 0.0356(3) 0.0454(3) 0.0461(3) -0.0034(2) 0.0235(2) -0.0005(2) Zn2 0.0366(3) 0.0529(3) 0.0441(3) 0.0024(2) 0.0227(2) -0.0017(2) C1 0.042(2) 0.060(3) 0.070(3) -0.004(2) 0.033(2) 0.007(2) C2 0.041(2) 0.057(3) 0.084(4) -0.002(3) 0.023(2) 0.019(2) C3 0.055(3) 0.057(3) 0.071(3) 0.016(2) 0.021(3) 0.022(2) C4 0.050(2) 0.055(3) 0.055(3) 0.008(2) 0.027(2) 0.009(2) C5 0.0291(18) 0.040(2) 0.044(2) -0.0014(17) 0.0161(17) 0.0025(17) C6 0.034(2) 0.040(2) 0.041(2) -0.0012(18) 0.0172(17) -0.0026(17) C7 0.0315(19) 0.041(2) 0.041(2) -0.0135(17) 0.0180(16) -0.0063(16) C8 0.0310(18) 0.042(2) 0.038(2) 0.0039(17) 0.0158(16) -0.0011(17) C9 0.056(3) 0.062(3) 0.053(3) 0.013(2) 0.030(2) 0.007(2) C10 0.073(3) 0.072(3) 0.058(3) 0.027(3) 0.032(3) 0.019(3) C11 0.043(2) 0.062(3) 0.065(3) 0.014(2) 0.014(2) 0.019(2) C12 0.041(2) 0.057(3) 0.065(3) 0.007(2) 0.027(2) 0.012(2) C13 0.052(3) 0.063(3) 0.072(3) 0.012(2) 0.039(2) 0.015(2) N1 0.0336(17) 0.0397(18) 0.055(2) 0.0000(15) 0.0225(16) 0.0049(15) N2 0.0310(16) 0.0447(19) 0.0435(19) -0.0063(16) 0.0160(14) 0.0027(14) N3 0.0303(15) 0.0397(17) 0.0424(18) 0.0037(15) 0.0155(14) 0.0082(14) N4 0.0323(16) 0.0444(18) 0.0428(19) 0.0042(15) 0.0190(14) 0.0057(15) N5 0.0353(17) 0.054(2) 0.056(2) 0.0018(16) 0.0282(16) 0.0039(16) N6 0.053(2) 0.068(3) 0.066(3) -0.020(2) 0.029(2) -0.004(2) N7 0.067(3) 0.076(3) 0.057(3) -0.015(2) 0.035(2) -0.003(2) N8 0.112(4) 0.128(5) 0.115(5) -0.037(4) 0.074(4) 0.011(4) N9 0.0319(17) 0.054(2) 0.046(2) -0.0038(16) 0.0229(15) -0.0022(15) N10 0.0397(19) 0.063(2) 0.047(2) -0.0017(18) 0.0232(17) -0.0001(17) N11 0.077(3) 0.132(5) 0.066(3) 0.000(3) 0.046(3) -0.005(3) N12 0.0369(18) 0.046(2) 0.070(2) 0.0006(18) 0.0348(18) 0.0034(15) N13 0.041(2) 0.064(3) 0.073(3) 0.001(2) 0.0366(19) 0.0039(19) N14 0.088(4) 0.062(3) 0.149(5) -0.033(3) 0.071(4) -0.008(3) _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 N6 2.007(4) . ? Zn1 N5 2.028(3) . ? Zn1 N9 2.090(3) . ? Zn1 N1 2.145(3) . ? Zn1 N2 2.161(3) . ? Zn2 N12 1.992(4) . ? Zn2 N9 2.026(3) 3_576 ? Zn2 N4 2.054(3) . ? Zn2 N3 2.098(3) . ? Zn2 N12 2.338(3) 3_476 ? C1 N1 1.345(5) . ? C1 C2 1.374(7) . ? C2 C3 1.352(8) . ? C3 C4 1.400(6) . ? C4 C5 1.388(6) . ? C5 N1 1.354(5) . ? C5 C6 1.477(5) . ? C6 N2 1.281(5) . ? C6 C13 1.494(6) . ? C7 N5 1.329(5) . ? C7 N3 1.351(5) . ? C7 C8 1.486(5) . ? C8 N4 1.349(5) . ? C8 C9 1.393(6) . ? C9 C10 1.397(6) . ? C10 C11 1.352(7) . ? C11 C12 1.370(7) . ? C12 N4 1.347(5) . ? N2 N3 1.389(4) . ? N6 N7 1.187(6) . ? N7 N8 1.150(6) . ? N9 N10 1.212(5) . ? N9 Zn2 2.026(3) 3_576 ? N10 N11 1.122(6) . ? N12 N13 1.215(5) . ? N12 Zn2 2.338(3) 3_476 ? N13 N14 1.134(6) . ? 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 N6 Zn1 N5 102.81(16) . . ? N6 Zn1 N9 104.24(15) . . ? N5 Zn1 N9 103.98(13) . . ? N6 Zn1 N1 99.14(16) . . ? N5 Zn1 N1 147.69(14) . . ? N9 Zn1 N1 93.12(13) . . ? N6 Zn1 N2 120.25(15) . . ? N5 Zn1 N2 74.72(13) . . ? N9 Zn1 N2 134.86(12) . . ? N1 Zn1 N2 73.81(12) . . ? N12 Zn2 N9 121.07(15) . 3_576 ? N12 Zn2 N4 115.31(14) . . ? N9 Zn2 N4 121.01(13) 3_576 . ? N12 Zn2 N3 110.35(13) . . ? N9 Zn2 N3 96.02(13) 3_576 . ? N4 Zn2 N3 79.22(12) . . ? N12 Zn2 N12 74.99(16) . 3_476 ? N9 Zn2 N12 87.68(13) 3_576 3_476 ? N4 Zn2 N12 91.11(13) . 3_476 ? N3 Zn2 N12 170.22(13) . 3_476 ? N1 C1 C2 122.3(4) . . ? C3 C2 C1 119.6(4) . . ? C2 C3 C4 119.7(5) . . ? C5 C4 C3 118.1(5) . . ? N1 C5 C4 121.7(4) . . ? N1 C5 C6 116.1(3) . . ? C4 C5 C6 122.2(4) . . ? N2 C6 C5 113.6(4) . . ? N2 C6 C13 128.1(4) . . ? C5 C6 C13 118.3(4) . . ? N5 C7 N3 122.8(4) . . ? N5 C7 C8 121.7(4) . . ? N3 C7 C8 115.5(3) . . ? N4 C8 C9 122.1(4) . . ? N4 C8 C7 115.3(3) . . ? C9 C8 C7 122.6(4) . . ? C8 C9 C10 117.5(4) . . ? C11 C10 C9 120.5(4) . . ? C10 C11 C12 119.0(4) . . ? N4 C12 C11 122.8(4) . . ? C1 N1 C5 118.5(4) . . ? C1 N1 Zn1 125.1(3) . . ? C5 N1 Zn1 116.1(2) . . ? C6 N2 N3 123.8(3) . . ? C6 N2 Zn1 120.0(3) . . ? N3 N2 Zn1 116.2(2) . . ? C7 N3 N2 109.6(3) . . ? C7 N3 Zn2 113.2(2) . . ? N2 N3 Zn2 136.2(3) . . ? C12 N4 C8 118.2(3) . . ? C12 N4 Zn2 126.6(3) . . ? C8 N4 Zn2 115.3(2) . . ? C7 N5 Zn1 116.2(3) . . ? N7 N6 Zn1 123.0(3) . . ? N8 N7 N6 178.7(6) . . ? N10 N9 Zn2 117.2(3) . 3_576 ? N10 N9 Zn1 117.6(3) . . ? Zn2 N9 Zn1 125.15(17) 3_576 . ? N11 N10 N9 179.0(5) . . ? N13 N12 Zn2 128.5(3) . . ? N13 N12 Zn2 124.4(3) . 3_476 ? Zn2 N12 Zn2 105.01(16) . 3_476 ? N14 N13 N12 175.8(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.884 _refine_diff_density_min -0.994 _refine_diff_density_rms 0.090 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 656074' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H13 N15 O Zn2' _chemical_formula_weight 514.11 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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5173(3) _cell_length_b 10.0830(3) _cell_length_c 19.5632(7) _cell_angle_alpha 90.00 _cell_angle_beta 116.8350(14) _cell_angle_gamma 90.00 _cell_volume 1851.18(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16391 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.103 _exptl_crystal_description Block _exptl_crystal_colour 'Light yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.845 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 2.635 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.689 _exptl_absorpt_correction_T_max 0.907 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _exptl_special_details ; Problems: Isolated Oxygen Atom (H-atoms Missing ?) OW Short Inter D...A Contact OW N15 1.93 Ang. Short Inter D...A Contact OW N14 2.86 Ang. Response: The solvent hydrogens can not be located due to the limited quality of the data and the problem of Short Inter D...A Contact +- may due to the heavy disorder in azido ligand in the structure Problem: diffrn_measured_fraction_theta_full Low 0.96 Response: The limited quality of the crystals gives rise to the weak diffraction,leading to the relatively low data completeness Problem: Large Non-Solvent N Ueq(max)/Ueq(min) 6.21 Ratio Response: It arises from the heavy disorder in azido ligand Problem: Check Low Ueq as Compared to Neighbors for N14 Response: It arises from the heavy disorder in azido ligand ; _diffrn_ambient_temperature 293(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 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30027 _diffrn_reflns_av_R_equivalents 0.1348 _diffrn_reflns_av_sigmaI/netI 0.1383 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.10 _reflns_number_total 3905 _reflns_number_gt 1869 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0446P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3905 _refine_ls_number_parameters 290 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1297 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.886 _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 C1 C 0.5429(5) 0.2063(5) 0.1544(3) 0.0593(15) Uani 1 1 d . . . H1A H 0.5982 0.2206 0.1290 0.071 Uiso 1 1 calc R . . C2 C 0.5807(5) 0.2684(6) 0.2235(3) 0.0666(16) Uani 1 1 d . . . H2A H 0.6604 0.3231 0.2448 0.080 Uiso 1 1 calc R . . C3 C 0.4981(6) 0.2478(6) 0.2599(3) 0.0719(17) Uani 1 1 d . . . H3A H 0.5207 0.2899 0.3063 0.086 Uiso 1 1 calc R . . C4 C 0.3826(5) 0.1656(5) 0.2287(3) 0.0597(15) Uani 1 1 d . . . H4A H 0.3268 0.1509 0.2537 0.072 Uiso 1 1 calc R . . C5 C 0.3499(5) 0.1050(5) 0.1596(2) 0.0424(12) Uani 1 1 d . . . C6 C 0.2287(4) 0.0108(4) 0.1226(2) 0.0382(11) Uani 1 1 d . . . C7 C 0.0871(5) -0.2233(5) -0.0219(3) 0.0449(12) Uani 1 1 d . . . C8 C -0.0410(4) -0.3104(5) -0.0433(3) 0.0457(12) Uani 1 1 d . . . C9 C -0.0872(5) -0.3995(6) -0.1038(3) 0.0604(15) Uani 1 1 d . . . H9A H -0.0391 -0.4071 -0.1335 0.072 Uiso 1 1 calc R . . C10 C -0.2045(6) -0.4763(6) -0.1191(4) 0.0713(16) Uani 1 1 d . . . H10B H -0.2378 -0.5361 -0.1596 0.086 Uiso 1 1 calc R . . C11 C -0.2724(5) -0.4633(6) -0.0734(3) 0.0676(16) Uani 1 1 d . . . H11A H -0.3519 -0.5147 -0.0824 0.081 Uiso 1 1 calc R . . C12 C -0.2205(5) -0.3729(5) -0.0142(3) 0.0608(15) Uani 1 1 d . . . H12A H -0.2662 -0.3653 0.0167 0.073 Uiso 1 1 calc R . . N1 N 0.4301(4) 0.1263(4) 0.1222(2) 0.0429(10) Uani 1 1 d . . . N2 N 0.2286(4) -0.0590(4) 0.0637(2) 0.0406(10) Uani 1 1 d . . . N3 N 0.1131(4) -0.1448(4) 0.0360(2) 0.0423(10) Uani 1 1 d . . . N4 N -0.1080(4) -0.2959(4) 0.0009(2) 0.0462(10) Uani 1 1 d . . . N5 N 0.1328(4) -0.0045(4) 0.1483(2) 0.0514(11) Uani 1 1 d . . . N6 N 0.1625(4) -0.2351(4) -0.0616(2) 0.0644(13) Uani 1 1 d . . . N7 N 0.2035(3) 0.0827(4) -0.07990(19) 0.0425(10) Uani 1 1 d . . . N8 N 0.2227(4) 0.0715(5) -0.1372(3) 0.0611(12) Uani 1 1 d . . . N9 N 0.2421(6) 0.0623(7) -0.1896(3) 0.109(2) Uani 1 1 d . . . N10 N 0.4739(4) -0.1288(4) 0.0081(2) 0.0444(10) Uani 1 1 d . . . N11 N 0.5038(5) -0.2323(6) 0.0421(3) 0.0614(13) Uani 1 1 d . . . N12 N 0.5341(6) -0.3318(6) 0.0745(4) 0.105(2) Uani 1 1 d . . . N13 N 0.0450(6) -0.2863(6) 0.1812(3) 0.0843(18) Uani 1 1 d D . . N14 N -0.004(2) -0.316(3) 0.2172(14) 0.083(6) Uani 0.60(4) 1 d PD A 1 N14' N -0.037(2) -0.359(2) 0.183(2) 0.086(9) Uani 0.40(4) 1 d PD A 2 N15 N -0.059(4) -0.343(4) 0.253(3) 0.25(2) Uani 0.60(4) 1 d PD A 1 N15' N -0.105(2) -0.428(3) 0.1982(17) 0.109(12) Uani 0.40(4) 1 d PD A 2 OW O -0.1661(11) -0.6103(16) 0.1787(6) 0.360(7) Uani 1 1 d . . . Zn1 Zn 0.36295(5) 0.02422(6) 0.02123(3) 0.04320(19) Uani 1 1 d . . . Zn2 Zn -0.00813(5) -0.15449(6) 0.09580(3) 0.0475(2) Uani 1 1 d . . . 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 0.046(3) 0.080(4) 0.056(4) -0.015(3) 0.026(3) -0.011(3) C2 0.042(3) 0.077(4) 0.070(4) -0.019(3) 0.016(3) -0.015(3) C3 0.070(4) 0.091(5) 0.055(4) -0.025(3) 0.028(3) -0.015(4) C4 0.054(3) 0.083(4) 0.047(3) -0.019(3) 0.027(3) -0.016(3) C5 0.037(3) 0.050(3) 0.041(3) -0.004(2) 0.018(2) 0.004(2) C6 0.030(2) 0.044(3) 0.036(3) 0.002(2) 0.010(2) -0.002(2) C7 0.035(3) 0.054(3) 0.044(3) 0.003(3) 0.017(2) 0.001(3) C8 0.029(2) 0.050(4) 0.054(3) 0.003(3) 0.015(2) 0.000(2) C9 0.056(3) 0.069(4) 0.063(4) -0.017(3) 0.032(3) -0.015(3) C10 0.061(4) 0.063(4) 0.089(4) -0.020(3) 0.033(3) -0.018(3) C11 0.050(3) 0.056(4) 0.092(5) 0.003(4) 0.028(3) -0.017(3) C12 0.048(3) 0.065(4) 0.076(4) 0.000(3) 0.034(3) -0.011(3) N1 0.031(2) 0.057(3) 0.040(2) -0.009(2) 0.0153(19) -0.009(2) N2 0.031(2) 0.055(3) 0.036(2) -0.005(2) 0.0152(18) -0.006(2) N3 0.032(2) 0.055(3) 0.043(2) -0.001(2) 0.0199(19) -0.004(2) N4 0.032(2) 0.053(3) 0.058(3) 0.002(2) 0.024(2) 0.000(2) N5 0.032(2) 0.080(3) 0.048(2) 0.001(2) 0.023(2) -0.005(2) N6 0.052(3) 0.097(4) 0.064(3) -0.022(3) 0.044(2) -0.022(3) N7 0.034(2) 0.070(3) 0.033(2) 0.003(2) 0.0238(19) 0.004(2) N8 0.045(3) 0.079(4) 0.060(3) 0.004(3) 0.023(2) 0.006(2) N9 0.091(4) 0.188(7) 0.065(4) 0.000(4) 0.048(3) 0.016(4) N10 0.038(2) 0.051(3) 0.052(3) 0.004(2) 0.027(2) -0.002(2) N11 0.047(3) 0.072(4) 0.083(4) 0.000(3) 0.044(3) -0.005(3) N12 0.102(5) 0.086(5) 0.153(6) 0.029(4) 0.081(4) 0.008(4) N13 0.074(4) 0.105(5) 0.083(5) 0.043(3) 0.044(3) 0.009(3) N14 0.118(11) 0.110(13) 0.041(9) 0.032(9) 0.051(9) 0.046(9) N14' 0.081(14) 0.15(2) 0.053(17) 0.046(12) 0.052(12) 0.059(13) N15 0.32(3) 0.31(3) 0.27(4) 0.18(3) 0.26(3) 0.15(3) N15' 0.103(15) 0.14(2) 0.095(17) 0.020(15) 0.054(13) -0.015(12) OW 0.291(11) 0.60(2) 0.271(11) -0.225(13) 0.199(10) -0.157(15) Zn1 0.0327(3) 0.0599(4) 0.0417(3) -0.0027(3) 0.0209(3) -0.0026(3) Zn2 0.0351(3) 0.0681(4) 0.0464(4) 0.0075(3) 0.0247(3) 0.0015(3) _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 C1 N1 1.334(6) . ? C1 C2 1.376(6) . ? C2 C3 1.365(7) . ? C3 C4 1.366(7) . ? C4 C5 1.378(6) . ? C5 N1 1.360(5) . ? C5 C6 1.489(6) . ? C6 N5 1.323(5) . ? C6 N2 1.350(5) . ? C7 N3 1.306(5) . ? C7 N6 1.343(5) . ? C7 C8 1.501(6) . ? C8 N4 1.349(5) . ? C8 C9 1.387(6) . ? C9 C10 1.371(7) . ? C10 C11 1.379(7) . ? C11 C12 1.379(7) . ? C12 N4 1.332(6) . ? N1 Zn1 2.050(3) . ? N2 N3 1.387(5) . ? N2 Zn1 2.110(3) . ? N3 Zn2 2.085(3) . ? N4 Zn2 2.196(4) . ? N5 Zn2 2.041(4) . ? N7 N8 1.230(5) . ? N7 Zn1 2.019(3) . ? N7 Zn2 2.066(3) 3 ? N8 N9 1.137(5) . ? N10 N11 1.200(6) . ? N10 Zn1 2.020(4) . ? N10 Zn1 2.297(4) 3_655 ? N11 N12 1.152(6) . ? N13 N14 1.089(8) . ? N13 N14' 1.143(10) . ? N13 Zn2 2.007(5) . ? N14 N15 1.116(8) . ? N14' N15' 1.132(10) . ? Zn1 N10 2.297(4) 3_655 ? Zn2 N7 2.066(3) 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 N1 C1 C2 122.6(5) . . ? C3 C2 C1 118.3(5) . . ? C2 C3 C4 120.4(5) . . ? C3 C4 C5 119.1(4) . . ? N1 C5 C4 121.1(4) . . ? N1 C5 C6 116.2(4) . . ? C4 C5 C6 122.7(4) . . ? N5 C6 N2 123.8(4) . . ? N5 C6 C5 121.4(4) . . ? N2 C6 C5 114.7(4) . . ? N3 C7 N6 127.5(4) . . ? N3 C7 C8 114.0(4) . . ? N6 C7 C8 118.5(4) . . ? N4 C8 C9 122.3(4) . . ? N4 C8 C7 114.9(4) . . ? C9 C8 C7 122.8(4) . . ? C10 C9 C8 119.1(5) . . ? C9 C10 C11 118.9(5) . . ? C10 C11 C12 118.9(5) . . ? N4 C12 C11 123.1(5) . . ? C1 N1 C5 118.5(4) . . ? C1 N1 Zn1 127.1(3) . . ? C5 N1 Zn1 114.3(3) . . ? C6 N2 N3 108.7(3) . . ? C6 N2 Zn1 112.7(3) . . ? N3 N2 Zn1 135.9(3) . . ? C7 N3 N2 121.4(3) . . ? C7 N3 Zn2 121.1(3) . . ? N2 N3 Zn2 117.4(3) . . ? C12 N4 C8 117.6(4) . . ? C12 N4 Zn2 127.1(3) . . ? C8 N4 Zn2 115.1(3) . . ? C6 N5 Zn2 113.6(3) . . ? N8 N7 Zn1 117.4(3) . . ? N8 N7 Zn2 117.1(3) . 3 ? Zn1 N7 Zn2 125.41(16) . 3 ? N9 N8 N7 179.1(6) . . ? N11 N10 Zn1 128.0(3) . . ? N11 N10 Zn1 119.9(3) . 3_655 ? Zn1 N10 Zn1 102.74(18) . 3_655 ? N12 N11 N10 179.0(5) . . ? N14 N13 N14' 38.3(10) . . ? N14 N13 Zn2 133.2(10) . . ? N14' N13 Zn2 121.4(17) . . ? N13 N14 N15 178(2) . . ? N15' N14' N13 169(4) . . ? N7 Zn1 N10 111.75(16) . . ? N7 Zn1 N1 124.76(15) . . ? N10 Zn1 N1 122.58(15) . . ? N7 Zn1 N2 95.41(13) . . ? N10 Zn1 N2 105.92(15) . . ? N1 Zn1 N2 79.66(14) . . ? N7 Zn1 N10 90.26(14) . 3_655 ? N10 Zn1 N10 77.26(18) . 3_655 ? N1 Zn1 N10 92.26(14) . 3_655 ? N2 Zn1 N10 171.82(14) . 3_655 ? N13 Zn2 N5 101.9(2) . . ? N13 Zn2 N7 104.00(17) . 3 ? N5 Zn2 N7 105.25(15) . 3 ? N13 Zn2 N3 119.14(17) . . ? N5 Zn2 N3 76.03(14) . . ? N7 Zn2 N3 135.85(14) 3 . ? N13 Zn2 N4 97.0(2) . . ? N5 Zn2 N4 150.27(13) . . ? N7 Zn2 N4 92.08(14) 3 . ? N3 Zn2 N4 74.74(14) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.538 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.078 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 656075' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H10 N14 S Zn2' _chemical_formula_weight 501.13 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.3383(4) _cell_length_b 13.3717(4) _cell_length_c 17.5628(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.7236(16) _cell_angle_gamma 90.00 _cell_volume 3539.21(19) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15939 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour 'Light yellow' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.881 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 2.861 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.711 _exptl_absorpt_correction_T_max 0.814 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _exptl_special_details ; Problem: _diffrn_measured_fraction_theta_full Low 0.93 Response: Because of the limited quality, the crystal scattered weakly,giving the relatively low data completeness. Problem: Large Non-Solvent N Ueq(max)/Ueq(min) 3.86 Ratio Response: It arises from the large Ueq of terminal N11 atom of the azido bridge. ; _diffrn_ambient_temperature 293(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 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29473 _diffrn_reflns_av_R_equivalents 0.1231 _diffrn_reflns_av_sigmaI/netI 0.1260 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3753 _reflns_number_gt 1894 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0509P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3753 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1261 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1083 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_restrained_S_all 0.911 _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 C1 C 0.0705(4) 0.8806(4) -0.0407(3) 0.0493(14) Uani 1 1 d . . . H1A H 0.1109 0.9109 -0.0015 0.059 Uiso 1 1 calc R . . C2 C 0.0135(4) 0.9398(4) -0.0895(4) 0.0602(16) Uani 1 1 d . . . H2A H 0.0159 1.0090 -0.0844 0.072 Uiso 1 1 calc R . . C3 C -0.0460(4) 0.8967(5) -0.1449(4) 0.0684(18) Uani 1 1 d . . . H3A H -0.0858 0.9361 -0.1785 0.082 Uiso 1 1 calc R . . C4 C -0.0488(4) 0.7933(4) -0.1526(3) 0.0566(16) Uani 1 1 d . . . H4A H -0.0904 0.7629 -0.1909 0.068 Uiso 1 1 calc R . . C5 C 0.0117(3) 0.7363(4) -0.1021(3) 0.0378(13) Uani 1 1 d . . . C6 C 0.0144(3) 0.6247(4) -0.1057(3) 0.0345(12) Uani 1 1 d . . . C7 C 0.1390(3) 0.4303(4) -0.0086(3) 0.0372(12) Uani 1 1 d . . . C8 C 0.2023(3) 0.4660(4) 0.0579(3) 0.0365(12) Uani 1 1 d . . . C9 C 0.2761(4) 0.5614(4) 0.1497(3) 0.0575(16) Uani 1 1 d . . . H9A H 0.2943 0.6211 0.1748 0.069 Uiso 1 1 calc R . . C10 C 0.3041(5) 0.4732(5) 0.1784(3) 0.075(2) Uani 1 1 d . . . H10A H 0.3435 0.4644 0.2250 0.090 Uiso 1 1 calc R . . C11 C 0.1379(4) 0.3209(4) -0.0250(3) 0.0552(15) Uani 1 1 d . . . H11A H 0.0936 0.3068 -0.0700 0.083 Uiso 1 1 calc R . . H11B H 0.1242 0.2850 0.0186 0.083 Uiso 1 1 calc R . . H11C H 0.1950 0.3005 -0.0342 0.083 Uiso 1 1 calc R . . N1 N 0.0712(3) 0.7805(3) -0.0465(2) 0.0368(10) Uani 1 1 d . . . N2 N 0.0788(2) 0.5839(3) -0.0501(2) 0.0325(9) Uani 1 1 d . . . N3 N 0.0824(3) 0.4821(3) -0.0559(2) 0.0365(10) Uani 1 1 d . . . N4 N 0.2188(3) 0.5585(3) 0.0808(2) 0.0388(10) Uani 1 1 d . . . N5 N -0.0404(3) 0.5731(3) -0.1566(2) 0.0415(10) Uani 1 1 d . . . N6 N 0.2455(3) 0.7982(3) 0.0703(2) 0.0394(10) Uani 1 1 d . . . N7 N 0.2796(3) 0.8158(3) 0.1366(3) 0.0421(11) Uani 1 1 d . . . N8 N 0.3142(4) 0.8327(4) 0.1989(3) 0.0701(15) Uani 1 1 d . . . N9 N 0.0747(3) 0.6892(3) 0.1182(2) 0.0396(10) Uani 1 1 d . . . N10 N 0.0681(3) 0.7679(4) 0.1460(3) 0.0475(12) Uani 1 1 d . . . N11 N 0.0641(4) 0.8439(4) 0.1727(3) 0.0841(18) Uani 1 1 d . . . N12 N -0.0869(3) 0.6008(3) 0.2194(2) 0.0502(12) Uani 1 1 d . . . N13 N -0.1646(4) 0.6006(4) 0.1931(3) 0.0661(16) Uani 1 1 d . . . N14 N -0.2382(4) 0.5997(6) 0.1665(4) 0.124(3) Uani 1 1 d . . . Zn1 Zn 0.15839(4) 0.68444(4) 0.02470(3) 0.03810(19) Uani 1 1 d . . . Zn2 Zn 0.01520(4) 0.57272(5) 0.16277(4) 0.0453(2) Uani 1 1 d . . . S1 S 0.26011(11) 0.37976(11) 0.12089(9) 0.0607(4) Uani 1 1 d . . . 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 0.055(4) 0.041(4) 0.050(4) -0.005(3) 0.002(3) 0.001(3) C2 0.073(4) 0.034(4) 0.065(4) 0.005(3) -0.009(4) 0.013(3) C3 0.073(5) 0.050(4) 0.071(5) 0.012(3) -0.016(4) 0.027(4) C4 0.063(4) 0.055(4) 0.043(4) -0.003(3) -0.013(3) 0.011(3) C5 0.037(3) 0.043(3) 0.034(3) 0.007(3) 0.006(3) 0.007(3) C6 0.036(3) 0.036(3) 0.034(3) -0.001(3) 0.012(3) 0.005(3) C7 0.032(3) 0.039(3) 0.042(3) 0.006(3) 0.009(3) 0.008(3) C8 0.036(3) 0.038(3) 0.036(3) 0.003(2) 0.008(3) 0.003(2) C9 0.077(4) 0.045(4) 0.042(3) -0.003(3) -0.013(3) 0.010(3) C10 0.109(6) 0.064(4) 0.040(4) 0.002(3) -0.021(4) 0.015(4) C11 0.061(4) 0.044(4) 0.057(4) -0.005(3) 0.001(3) 0.007(3) N1 0.041(3) 0.036(3) 0.031(2) -0.002(2) 0.002(2) 0.002(2) N2 0.034(2) 0.033(3) 0.028(2) -0.0039(18) -0.0002(19) 0.0018(19) N3 0.035(2) 0.037(3) 0.038(2) -0.005(2) 0.008(2) 0.001(2) N4 0.043(3) 0.043(3) 0.030(2) 0.000(2) 0.003(2) 0.002(2) N5 0.045(3) 0.040(3) 0.036(3) -0.005(2) -0.001(2) -0.002(2) N6 0.038(3) 0.039(3) 0.038(3) -0.001(2) -0.001(2) -0.008(2) N7 0.046(3) 0.042(3) 0.039(3) -0.002(2) 0.009(2) -0.005(2) N8 0.074(4) 0.083(4) 0.046(3) -0.005(3) -0.008(3) -0.008(3) N9 0.047(3) 0.034(3) 0.040(3) -0.006(2) 0.014(2) -0.004(2) N10 0.054(3) 0.042(3) 0.046(3) -0.001(3) 0.010(2) -0.006(3) N11 0.117(5) 0.059(4) 0.080(4) -0.006(3) 0.027(4) 0.000(4) N12 0.045(3) 0.069(3) 0.037(3) -0.002(2) 0.007(2) 0.005(3) N13 0.052(4) 0.093(4) 0.059(4) 0.023(3) 0.023(3) 0.012(3) N14 0.053(4) 0.220(9) 0.101(5) 0.063(5) 0.016(4) 0.020(5) Zn1 0.0406(4) 0.0337(4) 0.0349(3) -0.0014(3) -0.0061(3) -0.0009(3) Zn2 0.0465(4) 0.0428(4) 0.0469(4) -0.0042(3) 0.0092(3) -0.0049(3) S1 0.0795(11) 0.0459(9) 0.0480(9) 0.0033(7) -0.0113(8) 0.0157(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.342(6) . ? C1 C2 1.359(7) . ? C2 C3 1.333(8) . ? C3 C4 1.390(8) . ? C4 C5 1.386(7) . ? C5 N1 1.344(6) . ? C5 C6 1.495(7) . ? C6 N5 1.303(6) . ? C6 N2 1.367(6) . ? C7 N3 1.287(6) . ? C7 C8 1.453(7) . ? C7 C11 1.490(7) . ? C8 N4 1.311(6) . ? C8 S1 1.725(5) . ? C9 C10 1.322(7) . ? C9 N4 1.356(6) . ? C10 S1 1.669(6) . ? N1 Zn1 2.092(4) . ? N2 N3 1.367(5) . ? N2 Zn1 2.104(4) . ? N3 Zn2 2.292(4) 5_565 ? N4 Zn1 2.080(4) . ? N5 Zn2 1.995(4) 5_565 ? N6 N7 1.207(6) . ? N6 Zn1 2.084(4) . ? N6 Zn1 2.434(4) 7_565 ? N7 N8 1.146(6) . ? N9 N10 1.172(6) . ? N9 Zn2 2.035(4) . ? N9 Zn1 2.265(4) . ? N10 N11 1.126(6) . ? N12 N13 1.196(6) . ? N12 Zn2 2.040(4) . ? N12 Zn2 2.188(4) 2 ? N13 N14 1.138(7) . ? Zn1 N6 2.434(4) 7_565 ? Zn2 N5 1.995(4) 5_565 ? Zn2 N12 2.188(4) 2 ? Zn2 N3 2.292(4) 5_565 ? 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 C1 C2 123.1(5) . . ? C3 C2 C1 118.7(5) . . ? C2 C3 C4 120.4(6) . . ? C5 C4 C3 118.7(5) . . ? N1 C5 C4 120.5(5) . . ? N1 C5 C6 116.7(4) . . ? C4 C5 C6 122.8(5) . . ? N5 C6 N2 124.5(4) . . ? N5 C6 C5 122.5(5) . . ? N2 C6 C5 112.9(4) . . ? N3 C7 C8 127.7(5) . . ? N3 C7 C11 114.9(5) . . ? C8 C7 C11 117.4(5) . . ? N4 C8 C7 128.2(5) . . ? N4 C8 S1 112.7(4) . . ? C7 C8 S1 118.9(4) . . ? C10 C9 N4 115.2(5) . . ? C9 C10 S1 111.7(5) . . ? C1 N1 C5 118.6(4) . . ? C1 N1 Zn1 125.5(4) . . ? C5 N1 Zn1 115.9(3) . . ? C6 N2 N3 112.2(4) . . ? C6 N2 Zn1 116.7(3) . . ? N3 N2 Zn1 131.0(3) . . ? C7 N3 N2 121.3(4) . . ? C7 N3 Zn2 128.0(4) . 5_565 ? N2 N3 Zn2 110.5(3) . 5_565 ? C8 N4 C9 110.9(4) . . ? C8 N4 Zn1 125.1(3) . . ? C9 N4 Zn1 123.8(4) . . ? C6 N5 Zn2 116.6(3) . 5_565 ? N7 N6 Zn1 130.1(3) . . ? N7 N6 Zn1 115.7(3) . 7_565 ? Zn1 N6 Zn1 103.49(16) . 7_565 ? N8 N7 N6 178.1(5) . . ? N10 N9 Zn2 116.5(3) . . ? N10 N9 Zn1 115.6(3) . . ? Zn2 N9 Zn1 127.8(2) . . ? N11 N10 N9 178.1(6) . . ? N13 N12 Zn2 127.8(4) . . ? N13 N12 Zn2 130.8(4) . 2 ? Zn2 N12 Zn2 97.66(19) . 2 ? N14 N13 N12 178.4(7) . . ? N4 Zn1 N6 102.23(16) . . ? N4 Zn1 N1 163.53(16) . . ? N6 Zn1 N1 94.24(17) . . ? N4 Zn1 N2 86.23(16) . . ? N6 Zn1 N2 164.23(15) . . ? N1 Zn1 N2 77.72(16) . . ? N4 Zn1 N9 86.69(15) . . ? N6 Zn1 N9 96.35(15) . . ? N1 Zn1 N9 91.73(15) . . ? N2 Zn1 N9 97.42(14) . . ? N4 Zn1 N6 97.37(14) . 7_565 ? N6 Zn1 N6 76.51(16) . 7_565 ? N1 Zn1 N6 86.18(14) . 7_565 ? N2 Zn1 N6 89.31(14) . 7_565 ? N9 Zn1 N6 172.37(14) . 7_565 ? N5 Zn2 N9 128.46(16) 5_565 . ? N5 Zn2 N12 112.40(17) 5_565 . ? N9 Zn2 N12 119.12(17) . . ? N5 Zn2 N12 98.71(17) 5_565 2 ? N9 Zn2 N12 92.89(17) . 2 ? N12 Zn2 N12 78.7(2) . 2 ? N5 Zn2 N3 75.31(16) 5_565 5_565 ? N9 Zn2 N3 101.57(15) . 5_565 ? N12 Zn2 N3 90.84(16) . 5_565 ? N12 Zn2 N3 165.05(15) 2 5_565 ? C10 S1 C8 89.4(3) . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.503 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.092 #===END