data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Baolong, Li' _publ_contact_author_email libaolong@suda.edu.cn _publ_section_title ; A polythreading coordination array formed from 2D grid networks and 1D chains ; _publ_author_name 'Li Baolong' data_Zn-btp-Cl-phth _database_code_depnum_ccdc_archive 'CCDC 798100' #TrackingRef 'ZnbtpCIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H28 Cl N12 O7 Zn2' _chemical_formula_weight 786.79 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' Cl Cl 0.1484 0.1585 '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 10.283(3) _cell_length_b 10.282(3) _cell_length_c 17.380(5) _cell_angle_alpha 93.327(4) _cell_angle_beta 98.686(5) _cell_angle_gamma 111.005(7) _cell_volume 1683.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6421 _cell_measurement_theta_min 3.0043 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 802 _exptl_absorpt_coefficient_mu 1.566 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4340 _exptl_absorpt_correction_T_max 0.7448 _exptl_absorpt_process_details Empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16475 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6124 _reflns_number_gt 5151 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0884P)^2^+2.4132P] 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 6124 _refine_ls_number_parameters 454 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1683 _refine_ls_wR_factor_gt 0.1567 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.090 _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 0.51969(5) 0.11066(5) 0.19810(3) 0.03403(18) Uani 1 1 d . . . Zn2 Zn 0.88008(6) 0.43526(6) 0.62337(3) 0.0448(2) Uani 1 1 d . . . Cl1 Cl 1.06318(19) 0.59940(18) 0.70044(12) 0.0806(5) Uani 1 1 d . . . O1 O 0.5221(4) 0.2844(3) 0.15742(17) 0.0413(8) Uani 1 1 d . . . O2 O 0.5223(4) 0.1644(3) 0.04727(19) 0.0455(8) Uani 1 1 d . . . O3 O 0.5646(4) 0.1185(4) 0.31172(19) 0.0522(9) Uani 1 1 d . . . O4 O 0.3730(4) 0.1539(4) 0.3338(2) 0.0593(10) Uani 1 1 d . . . O5 O 0.9234(4) 0.3082(4) 0.5538(2) 0.0531(9) Uani 1 1 d . . . O6 O 0.9360(4) 0.2041(4) 0.6605(2) 0.0601(10) Uani 1 1 d . . . O7 O 0.2331(12) 0.3103(11) 0.2670(7) 0.084(3) Uani 0.50 1 d PD . . O8 O 0.141(2) 0.2113(15) 0.1050(8) 0.139(7) Uani 0.50 1 d PD . . N1 N 0.1081(4) -0.1850(4) 0.1435(2) 0.0387(9) Uani 1 1 d . . . N2 N 0.1538(5) -0.2155(5) 0.0780(3) 0.0487(11) Uani 1 1 d . . . N3 N 0.3269(4) -0.0422(4) 0.1580(2) 0.0398(9) Uani 1 1 d . . . N4 N -0.1922(4) -0.0430(4) 0.1241(2) 0.0421(9) Uani 1 1 d . . . N5 N -0.1207(4) 0.0082(5) 0.1992(3) 0.0488(11) Uani 1 1 d . . . N6 N -0.3231(4) 0.0460(4) 0.1775(2) 0.0370(9) Uani 1 1 d . . . N7 N 0.6793(4) 0.5150(4) 0.4152(3) 0.0449(10) Uani 1 1 d . . . N8 N 0.6491(5) 0.6070(5) 0.4632(3) 0.0509(11) Uani 1 1 d . . . N9 N 0.7807(5) 0.5076(5) 0.5336(3) 0.0494(11) Uani 1 1 d . . . N10 N 0.4979(5) 0.7037(5) 0.2975(3) 0.0480(10) Uani 1 1 d . . . N11 N 0.4146(6) 0.6691(6) 0.2256(3) 0.0599(13) Uani 1 1 d . . . N12 N 0.2827(5) 0.6376(5) 0.3191(2) 0.0464(10) Uani 1 1 d . . . C1 C -0.0374(5) -0.2601(6) 0.1543(3) 0.0476(12) Uani 1 1 d . . . H1A H -0.0526 -0.2183 0.2019 0.057 Uiso 1 1 calc R . . H1B H -0.0510 -0.3571 0.1602 0.057 Uiso 1 1 calc R . . C2 C -0.1446(6) -0.2557(6) 0.0858(3) 0.0513(13) Uani 1 1 d . . . H2A H -0.2387 -0.3068 0.0959 0.062 Uiso 1 1 calc R . . H2B H -0.1333 -0.3047 0.0394 0.062 Uiso 1 1 calc R . . C3 C -0.1356(6) -0.1106(7) 0.0684(3) 0.0534(14) Uani 1 1 d . . . H3A H -0.0372 -0.0523 0.0694 0.064 Uiso 1 1 calc R . . H3B H -0.1877 -0.1174 0.0159 0.064 Uiso 1 1 calc R . . C5 C 0.2109(5) -0.0818(5) 0.1903(3) 0.0404(11) Uani 1 1 d . . . H5A H 0.2037 -0.0428 0.2383 0.049 Uiso 1 1 calc R . . C4 C 0.2846(6) -0.1276(6) 0.0894(3) 0.0455(12) Uani 1 1 d . . . H4A H 0.3439 -0.1238 0.0535 0.055 Uiso 1 1 calc R . . C6 C -0.2048(5) 0.0592(5) 0.2281(3) 0.0437(12) Uani 1 1 d . . . H6A H -0.1848 0.1012 0.2796 0.052 Uiso 1 1 calc R . . C7 C -0.3106(5) -0.0201(5) 0.1126(3) 0.0414(11) Uani 1 1 d . . . H7A H -0.3763 -0.0463 0.0659 0.050 Uiso 1 1 calc R . . C8 C 0.5098(5) 0.3903(4) 0.0405(2) 0.0306(9) Uani 1 1 d . . . C9 C 0.5502(5) 0.4056(5) -0.0322(3) 0.0373(10) Uani 1 1 d . . . H9A H 0.5839 0.3421 -0.0541 0.045 Uiso 1 1 calc R . . C10 C 0.5400(5) 0.5158(5) -0.0722(3) 0.0361(10) Uani 1 1 d . . . H10A H 0.5673 0.5258 -0.1209 0.043 Uiso 1 1 calc R . . C11 C 0.5194(5) 0.2699(5) 0.0832(3) 0.0350(10) Uani 1 1 d . . . C12 C 0.4893(5) 0.0594(5) 0.4304(2) 0.0322(9) Uani 1 1 d . . . C13 C 0.6028(5) 0.0195(5) 0.4544(3) 0.0419(11) Uani 1 1 d . . . H13A H 0.6719 0.0321 0.4236 0.050 Uiso 1 1 calc R . . C14 C 0.6144(5) -0.0390(5) 0.5237(3) 0.0396(11) Uani 1 1 d . . . H14A H 0.6915 -0.0646 0.5395 0.048 Uiso 1 1 calc R . . C15 C 0.4721(5) 0.1169(5) 0.3533(3) 0.0405(11) Uani 1 1 d . . . C16 C 0.6254(6) 0.4892(6) 0.3313(3) 0.0502(13) Uani 1 1 d . . . H16A H 0.5233 0.4620 0.3226 0.060 Uiso 1 1 calc R . . H16B H 0.6455 0.4109 0.3095 0.060 Uiso 1 1 calc R . . C17 C 0.6870(6) 0.6134(6) 0.2878(3) 0.0515(13) Uani 1 1 d . . . H17A H 0.7893 0.6421 0.2982 0.062 Uiso 1 1 calc R . . H17B H 0.6546 0.5830 0.2320 0.062 Uiso 1 1 calc R . . C18 C 0.6511(6) 0.7388(6) 0.3075(4) 0.0604(15) Uani 1 1 d . . . H18A H 0.6945 0.7782 0.3614 0.072 Uiso 1 1 calc R . . H18B H 0.6903 0.8095 0.2740 0.072 Uiso 1 1 calc R . . C19 C 0.7117(6) 0.5981(6) 0.5331(3) 0.0489(12) Uani 1 1 d . . . H19A H 0.7091 0.6493 0.5784 0.059 Uiso 1 1 calc R . . C20 C 0.7575(6) 0.4575(6) 0.4574(3) 0.0516(13) Uani 1 1 d . . . H20A H 0.7914 0.3925 0.4375 0.062 Uiso 1 1 calc R . . C21 C 0.2867(6) 0.6290(7) 0.2420(3) 0.0545(14) Uani 1 1 d . . . H21A H 0.2053 0.5973 0.2034 0.065 Uiso 1 1 calc R . . C22 C 0.4186(6) 0.6860(6) 0.3524(3) 0.0489(13) Uani 1 1 d . . . H22A H 0.4531 0.7046 0.4061 0.059 Uiso 1 1 calc R . . C23 C 0.9737(5) 0.1023(5) 0.5432(3) 0.0355(10) Uani 1 1 d . . . C24 C 0.9927(5) -0.0087(5) 0.5782(3) 0.0408(11) Uani 1 1 d . . . H24A H 0.9877 -0.0146 0.6309 0.049 Uiso 1 1 calc R . . C25 C 1.0190(5) -0.1107(5) 0.5351(3) 0.0409(11) Uani 1 1 d . . . H25A H 1.0318 -0.1851 0.5588 0.049 Uiso 1 1 calc R . . C26 C 0.9427(5) 0.2115(5) 0.5906(3) 0.0410(11) Uani 1 1 d . . . H1W H 0.266(12) 0.302(13) 0.226(4) 0.049 Uiso 0.50 1 d PD . . H2W H 0.168(9) 0.247(9) 0.281(7) 0.049 Uiso 0.50 1 d PD . . H3W H 0.187(11) 0.218(12) 0.151(3) 0.049 Uiso 0.50 1 d PD . . H4W H 0.087(12) 0.257(13) 0.110(9) 0.049 Uiso 0.50 1 d PD . . 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 0.0427(3) 0.0359(3) 0.0295(3) 0.0146(2) 0.0098(2) 0.0189(2) Zn2 0.0512(4) 0.0424(3) 0.0485(4) 0.0064(3) 0.0122(3) 0.0252(3) Cl1 0.0716(11) 0.0587(9) 0.0943(13) -0.0241(9) 0.0110(9) 0.0108(8) O1 0.066(2) 0.0374(17) 0.0292(17) 0.0148(14) 0.0123(15) 0.0259(16) O2 0.073(2) 0.0389(19) 0.0348(17) 0.0122(15) 0.0098(16) 0.0323(18) O3 0.061(2) 0.071(3) 0.0281(17) 0.0209(17) 0.0147(16) 0.023(2) O4 0.066(3) 0.075(3) 0.049(2) 0.028(2) 0.0074(18) 0.039(2) O5 0.075(3) 0.046(2) 0.053(2) 0.0087(17) 0.0177(19) 0.038(2) O6 0.081(3) 0.067(3) 0.044(2) -0.0007(18) 0.0128(19) 0.041(2) O7 0.106(9) 0.076(7) 0.090(7) 0.010(6) -0.015(7) 0.072(6) O8 0.181(16) 0.109(11) 0.059(6) -0.013(7) 0.059(9) -0.037(9) N1 0.036(2) 0.042(2) 0.039(2) 0.0037(18) 0.0085(17) 0.0151(18) N2 0.044(3) 0.052(3) 0.048(3) -0.008(2) 0.008(2) 0.017(2) N3 0.042(2) 0.040(2) 0.042(2) 0.0130(18) 0.0117(18) 0.0178(18) N4 0.041(2) 0.052(2) 0.039(2) 0.0110(19) 0.0096(18) 0.023(2) N5 0.043(2) 0.055(3) 0.047(2) 0.003(2) -0.0035(19) 0.021(2) N6 0.044(2) 0.038(2) 0.034(2) 0.0096(17) 0.0054(17) 0.0206(18) N7 0.048(2) 0.041(2) 0.052(3) 0.010(2) 0.015(2) 0.021(2) N8 0.059(3) 0.051(3) 0.054(3) 0.010(2) 0.013(2) 0.032(2) N9 0.059(3) 0.052(3) 0.049(3) 0.015(2) 0.020(2) 0.028(2) N10 0.054(3) 0.047(2) 0.053(3) 0.019(2) 0.018(2) 0.025(2) N11 0.071(3) 0.083(4) 0.043(3) 0.020(2) 0.015(2) 0.046(3) N12 0.055(3) 0.052(3) 0.045(2) 0.012(2) 0.013(2) 0.032(2) C1 0.044(3) 0.045(3) 0.059(3) 0.014(2) 0.018(2) 0.018(2) C2 0.042(3) 0.058(3) 0.053(3) -0.006(3) 0.007(2) 0.021(3) C3 0.050(3) 0.078(4) 0.043(3) 0.013(3) 0.014(2) 0.035(3) C5 0.046(3) 0.044(3) 0.039(3) 0.011(2) 0.012(2) 0.022(2) C4 0.050(3) 0.055(3) 0.039(3) 0.005(2) 0.014(2) 0.026(3) C6 0.046(3) 0.043(3) 0.042(3) 0.003(2) -0.003(2) 0.022(2) C7 0.041(3) 0.053(3) 0.036(3) 0.009(2) 0.004(2) 0.025(2) C8 0.037(2) 0.030(2) 0.028(2) 0.0120(17) 0.0065(18) 0.0147(19) C9 0.050(3) 0.039(2) 0.032(2) 0.0107(19) 0.011(2) 0.025(2) C10 0.050(3) 0.040(2) 0.027(2) 0.0133(19) 0.0143(19) 0.022(2) C11 0.038(2) 0.036(2) 0.035(2) 0.015(2) 0.0066(19) 0.016(2) C12 0.034(2) 0.034(2) 0.026(2) 0.0096(18) 0.0042(18) 0.0099(19) C13 0.042(3) 0.056(3) 0.034(2) 0.016(2) 0.016(2) 0.021(2) C14 0.036(3) 0.050(3) 0.039(3) 0.018(2) 0.009(2) 0.021(2) C15 0.049(3) 0.035(2) 0.029(2) 0.010(2) 0.002(2) 0.008(2) C16 0.050(3) 0.049(3) 0.050(3) 0.000(2) 0.005(2) 0.018(3) C17 0.040(3) 0.069(4) 0.047(3) 0.012(3) 0.014(2) 0.019(3) C18 0.053(3) 0.056(3) 0.072(4) 0.031(3) 0.021(3) 0.013(3) C19 0.059(3) 0.049(3) 0.048(3) 0.010(2) 0.014(2) 0.028(3) C20 0.061(3) 0.048(3) 0.062(4) 0.017(3) 0.023(3) 0.032(3) C21 0.062(4) 0.072(4) 0.041(3) 0.005(3) 0.005(3) 0.041(3) C22 0.060(3) 0.048(3) 0.041(3) 0.010(2) 0.013(2) 0.020(3) C23 0.032(2) 0.038(2) 0.038(2) 0.003(2) 0.0039(19) 0.016(2) C24 0.041(3) 0.045(3) 0.038(3) 0.007(2) 0.006(2) 0.019(2) C25 0.043(3) 0.039(3) 0.044(3) 0.007(2) 0.006(2) 0.020(2) C26 0.033(3) 0.040(3) 0.047(3) -0.004(2) 0.003(2) 0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.949(3) . ? Zn1 O1 1.953(3) . ? Zn1 N6 2.026(4) 1_655 ? Zn1 N3 2.027(4) . ? Zn2 O5 1.940(3) . ? Zn2 N12 2.014(4) 2_666 ? Zn2 N9 2.057(4) . ? Zn2 Cl1 2.2104(18) . ? O1 C11 1.285(5) . ? O2 C11 1.232(6) . ? O3 C15 1.275(6) . ? O4 C15 1.219(6) . ? O5 C26 1.270(6) . ? O6 C26 1.233(6) . ? O7 H1W 0.84(2) . ? O7 H2W 0.83(2) . ? O8 H3W 0.85(2) . ? O8 H4W 0.85(2) . ? N1 C5 1.320(6) . ? N1 N2 1.356(6) . ? N1 C1 1.464(6) . ? N2 C4 1.301(7) . ? N3 C5 1.335(6) . ? N3 C4 1.353(6) . ? N4 C7 1.310(6) . ? N4 N5 1.368(6) . ? N4 C3 1.464(7) . ? N5 C6 1.305(6) . ? N6 C7 1.329(6) . ? N6 C6 1.348(6) . ? N6 Zn1 2.026(4) 1_455 ? N7 C20 1.322(7) . ? N7 N8 1.373(6) . ? N7 C16 1.452(7) . ? N8 C19 1.311(7) . ? N9 C20 1.345(7) . ? N9 C19 1.358(7) . ? N10 C22 1.325(7) . ? N10 N11 1.353(6) . ? N10 C18 1.465(7) . ? N11 C21 1.312(7) . ? N12 C22 1.327(7) . ? N12 C21 1.346(7) . ? N12 Zn2 2.014(4) 2_666 ? C1 C2 1.510(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.513(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 H5A 0.9300 . ? C4 H4A 0.9300 . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C10 1.371(6) 2_665 ? C8 C9 1.389(6) . ? C8 C11 1.505(6) . ? C9 C10 1.390(6) . ? C9 H9A 0.9300 . ? C10 C8 1.371(6) 2_665 ? C10 H10A 0.9300 . ? C12 C13 1.387(6) . ? C12 C14 1.390(6) 2_656 ? C12 C15 1.507(6) . ? C13 C14 1.386(6) . ? C13 H13A 0.9300 . ? C14 C12 1.390(6) 2_656 ? C14 H14A 0.9300 . ? C16 C17 1.510(8) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.497(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C25 1.380(7) 2_756 ? C23 C24 1.383(7) . ? C23 C26 1.507(6) . ? C24 C25 1.382(7) . ? C24 H24A 0.9300 . ? C25 C23 1.380(7) 2_756 ? C25 H25A 0.9300 . ? 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 O3 Zn1 O1 116.47(15) . . ? O3 Zn1 N6 94.80(16) . 1_655 ? O1 Zn1 N6 116.10(15) . 1_655 ? O3 Zn1 N3 108.87(16) . . ? O1 Zn1 N3 108.90(15) . . ? N6 Zn1 N3 110.98(16) 1_655 . ? O5 Zn2 N12 120.62(18) . 2_666 ? O5 Zn2 N9 94.10(17) . . ? N12 Zn2 N9 98.16(17) 2_666 . ? O5 Zn2 Cl1 116.29(13) . . ? N12 Zn2 Cl1 110.29(14) 2_666 . ? N9 Zn2 Cl1 114.66(15) . . ? C11 O1 Zn1 108.4(3) . . ? C15 O3 Zn1 120.1(3) . . ? C26 O5 Zn2 109.9(3) . . ? H1W O7 H2W 124(10) . . ? H3W O8 H4W 106(10) . . ? C5 N1 N2 110.0(4) . . ? C5 N1 C1 128.7(4) . . ? N2 N1 C1 121.2(4) . . ? C4 N2 N1 103.2(4) . . ? C5 N3 C4 103.1(4) . . ? C5 N3 Zn1 129.7(3) . . ? C4 N3 Zn1 127.2(3) . . ? C7 N4 N5 110.1(4) . . ? C7 N4 C3 128.2(4) . . ? N5 N4 C3 121.7(4) . . ? C6 N5 N4 102.3(4) . . ? C7 N6 C6 103.1(4) . . ? C7 N6 Zn1 129.5(3) . 1_455 ? C6 N6 Zn1 127.4(3) . 1_455 ? C20 N7 N8 109.8(4) . . ? C20 N7 C16 128.7(5) . . ? N8 N7 C16 121.5(4) . . ? C19 N8 N7 103.2(4) . . ? C20 N9 C19 103.4(4) . . ? C20 N9 Zn2 124.1(4) . . ? C19 N9 Zn2 132.2(4) . . ? C22 N10 N11 110.0(5) . . ? C22 N10 C18 128.2(5) . . ? N11 N10 C18 121.4(5) . . ? C21 N11 N10 102.6(4) . . ? C22 N12 C21 103.1(4) . . ? C22 N12 Zn2 124.9(4) . 2_666 ? C21 N12 Zn2 131.2(4) . 2_666 ? N1 C1 C2 111.8(4) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 107.9 . . ? C1 C2 C3 115.5(5) . . ? C1 C2 H2A 108.4 . . ? C3 C2 H2A 108.4 . . ? C1 C2 H2B 108.4 . . ? C3 C2 H2B 108.4 . . ? H2A C2 H2B 107.5 . . ? N4 C3 C2 113.0(4) . . ? N4 C3 H3A 109.0 . . ? C2 C3 H3A 109.0 . . ? N4 C3 H3B 109.0 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? N1 C5 N3 109.5(4) . . ? N1 C5 H5A 125.3 . . ? N3 C5 H5A 125.3 . . ? N2 C4 N3 114.2(4) . . ? N2 C4 H4A 122.9 . . ? N3 C4 H4A 122.9 . . ? N5 C6 N6 114.6(4) . . ? N5 C6 H6A 122.7 . . ? N6 C6 H6A 122.7 . . ? N4 C7 N6 109.9(4) . . ? N4 C7 H7A 125.0 . . ? N6 C7 H7A 125.0 . . ? C10 C8 C9 119.6(4) 2_665 . ? C10 C8 C11 120.7(4) 2_665 . ? C9 C8 C11 119.8(4) . . ? C8 C9 C10 120.0(4) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C8 C10 C9 120.5(4) 2_665 . ? C8 C10 H10A 119.8 2_665 . ? C9 C10 H10A 119.8 . . ? O2 C11 O1 123.5(4) . . ? O2 C11 C8 120.6(4) . . ? O1 C11 C8 115.9(4) . . ? C13 C12 C14 119.4(4) . 2_656 ? C13 C12 C15 121.1(4) . . ? C14 C12 C15 119.5(4) 2_656 . ? C14 C13 C12 120.6(4) . . ? C14 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? C13 C14 C12 119.9(4) . 2_656 ? C13 C14 H14A 120.0 . . ? C12 C14 H14A 120.0 2_656 . ? O4 C15 O3 124.8(4) . . ? O4 C15 C12 120.2(5) . . ? O3 C15 C12 114.9(4) . . ? N7 C16 C17 114.2(4) . . ? N7 C16 H16A 108.7 . . ? C17 C16 H16A 108.7 . . ? N7 C16 H16B 108.7 . . ? C17 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C18 C17 C16 115.9(5) . . ? C18 C17 H17A 108.3 . . ? C16 C17 H17A 108.3 . . ? C18 C17 H17B 108.3 . . ? C16 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? N10 C18 C17 112.2(5) . . ? N10 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? N10 C18 H18B 109.2 . . ? C17 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? N8 C19 N9 114.0(5) . . ? N8 C19 H19A 123.0 . . ? N9 C19 H19A 123.0 . . ? N7 C20 N9 109.6(5) . . ? N7 C20 H20A 125.2 . . ? N9 C20 H20A 125.2 . . ? N11 C21 N12 114.6(5) . . ? N11 C21 H21A 122.7 . . ? N12 C21 H21A 122.7 . . ? N10 C22 N12 109.7(5) . . ? N10 C22 H22A 125.1 . . ? N12 C22 H22A 125.1 . . ? C25 C23 C24 119.8(4) 2_756 . ? C25 C23 C26 120.6(4) 2_756 . ? C24 C23 C26 119.7(4) . . ? C25 C24 C23 120.2(4) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C23 C25 C24 120.0(5) 2_756 . ? C23 C25 H25A 120.0 2_756 . ? C24 C25 H25A 120.0 . . ? O6 C26 O5 123.4(5) . . ? O6 C26 C23 120.7(5) . . ? O5 C26 C23 115.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Zn1 O1 C11 167.0(3) . . . . ? N6 Zn1 O1 C11 56.6(3) 1_655 . . . ? N3 Zn1 O1 C11 -69.5(3) . . . . ? O1 Zn1 O3 C15 77.3(4) . . . . ? N6 Zn1 O3 C15 -160.3(4) 1_655 . . . ? N3 Zn1 O3 C15 -46.2(4) . . . . ? N12 Zn2 O5 C26 -55.6(4) 2_666 . . . ? N9 Zn2 O5 C26 -157.6(3) . . . . ? Cl1 Zn2 O5 C26 82.3(3) . . . . ? C5 N1 N2 C4 0.3(5) . . . . ? C1 N1 N2 C4 179.2(4) . . . . ? O3 Zn1 N3 C5 36.4(4) . . . . ? O1 Zn1 N3 C5 -91.6(4) . . . . ? N6 Zn1 N3 C5 139.4(4) 1_655 . . . ? O3 Zn1 N3 C4 -145.3(4) . . . . ? O1 Zn1 N3 C4 86.8(4) . . . . ? N6 Zn1 N3 C4 -42.2(4) 1_655 . . . ? C7 N4 N5 C6 0.2(6) . . . . ? C3 N4 N5 C6 179.6(5) . . . . ? C20 N7 N8 C19 -0.5(6) . . . . ? C16 N7 N8 C19 178.2(5) . . . . ? O5 Zn2 N9 C20 4.3(5) . . . . ? N12 Zn2 N9 C20 -117.4(4) 2_666 . . . ? Cl1 Zn2 N9 C20 125.8(4) . . . . ? O5 Zn2 N9 C19 176.3(5) . . . . ? N12 Zn2 N9 C19 54.6(5) 2_666 . . . ? Cl1 Zn2 N9 C19 -62.3(5) . . . . ? C22 N10 N11 C21 -1.2(6) . . . . ? C18 N10 N11 C21 172.5(5) . . . . ? C5 N1 C1 C2 124.8(5) . . . . ? N2 N1 C1 C2 -53.8(6) . . . . ? N1 C1 C2 C3 -58.2(6) . . . . ? C7 N4 C3 C2 -107.5(6) . . . . ? N5 N4 C3 C2 73.3(6) . . . . ? C1 C2 C3 N4 -75.3(6) . . . . ? N2 N1 C5 N3 -0.6(5) . . . . ? C1 N1 C5 N3 -179.4(4) . . . . ? C4 N3 C5 N1 0.6(5) . . . . ? Zn1 N3 C5 N1 179.2(3) . . . . ? N1 N2 C4 N3 0.1(6) . . . . ? C5 N3 C4 N2 -0.4(6) . . . . ? Zn1 N3 C4 N2 -179.1(3) . . . . ? N4 N5 C6 N6 -0.7(6) . . . . ? C7 N6 C6 N5 0.8(6) . . . . ? Zn1 N6 C6 N5 -179.8(3) 1_455 . . . ? N5 N4 C7 N6 0.2(6) . . . . ? C3 N4 C7 N6 -179.1(5) . . . . ? C6 N6 C7 N4 -0.6(5) . . . . ? Zn1 N6 C7 N4 -179.9(3) 1_455 . . . ? C10 C8 C9 C10 0.1(8) 2_665 . . . ? C11 C8 C9 C10 179.3(4) . . . . ? C8 C9 C10 C8 -0.1(8) . . . 2_665 ? Zn1 O1 C11 O2 -3.3(6) . . . . ? Zn1 O1 C11 C8 175.6(3) . . . . ? C10 C8 C11 O2 158.1(5) 2_665 . . . ? C9 C8 C11 O2 -21.1(7) . . . . ? C10 C8 C11 O1 -20.9(6) 2_665 . . . ? C9 C8 C11 O1 159.9(4) . . . . ? C14 C12 C13 C14 -0.7(8) 2_656 . . . ? C15 C12 C13 C14 -177.1(5) . . . . ? C12 C13 C14 C12 0.7(8) . . . 2_656 ? Zn1 O3 C15 O4 -24.1(7) . . . . ? Zn1 O3 C15 C12 153.8(3) . . . . ? C13 C12 C15 O4 -178.7(5) . . . . ? C14 C12 C15 O4 4.8(7) 2_656 . . . ? C13 C12 C15 O3 3.3(7) . . . . ? C14 C12 C15 O3 -173.1(4) 2_656 . . . ? C20 N7 C16 C17 -114.1(6) . . . . ? N8 N7 C16 C17 67.5(6) . . . . ? N7 C16 C17 C18 -65.4(6) . . . . ? C22 N10 C18 C17 102.3(7) . . . . ? N11 N10 C18 C17 -70.1(6) . . . . ? C16 C17 C18 N10 -55.1(7) . . . . ? N7 N8 C19 N9 0.3(6) . . . . ? C20 N9 C19 N8 -0.1(6) . . . . ? Zn2 N9 C19 N8 -173.3(4) . . . . ? N8 N7 C20 N9 0.5(6) . . . . ? C16 N7 C20 N9 -178.1(5) . . . . ? C19 N9 C20 N7 -0.2(6) . . . . ? Zn2 N9 C20 N7 173.7(3) . . . . ? N10 N11 C21 N12 0.9(7) . . . . ? C22 N12 C21 N11 -0.3(7) . . . . ? Zn2 N12 C21 N11 -169.6(4) 2_666 . . . ? N11 N10 C22 N12 1.1(6) . . . . ? C18 N10 C22 N12 -172.0(5) . . . . ? C21 N12 C22 N10 -0.5(6) . . . . ? Zn2 N12 C22 N10 169.7(3) 2_666 . . . ? C25 C23 C24 C25 0.1(8) 2_756 . . . ? C26 C23 C24 C25 179.0(4) . . . . ? C23 C24 C25 C23 -0.1(8) . . . 2_756 ? Zn2 O5 C26 O6 -0.9(6) . . . . ? Zn2 O5 C26 C23 178.5(3) . . . . ? C25 C23 C26 O6 179.9(5) 2_756 . . . ? C24 C23 C26 O6 1.0(7) . . . . ? C25 C23 C26 O5 0.5(7) 2_756 . . . ? C24 C23 C26 O5 -178.4(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H1W O8 0.84(2) 2.25(10) 2.834(17) 127(10) . O8 H3W O7 0.85(2) 2.09(7) 2.834(17) 146(11) . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.132 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.099 ###====== data_Zn-btp-phth _database_code_depnum_ccdc_archive 'CCDC 798101' #TrackingRef 'ZnbtpCIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H22 N6 O7 Zn' _chemical_formula_weight 475.77 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 10.3742(3) _cell_length_b 10.9261(5) _cell_length_c 11.5914(11) _cell_angle_alpha 68.78(3) _cell_angle_beta 65.22(2) _cell_angle_gamma 62.77(2) _cell_volume 1036.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3335 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 1.235 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6718 _exptl_absorpt_correction_T_max 0.7903 _exptl_absorpt_process_details Empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8346 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_sigmaI/netI 0.1716 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 25.34 _reflns_number_total 3533 _reflns_number_gt 1712 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.1078P)^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 3533 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1260 _refine_ls_R_factor_gt 0.0717 _refine_ls_wR_factor_ref 0.2686 _refine_ls_wR_factor_gt 0.1868 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 -0.05877(11) 0.21877(10) 0.85065(10) 0.0358(4) Uani 1 1 d . . . O1 O 0.1132(7) 0.1047(6) 0.7292(6) 0.0385(16) Uani 1 1 d . . . O2 O 0.2097(7) 0.2619(7) 0.6974(7) 0.0503(18) Uani 1 1 d . . . O3 O -0.2046(7) 0.1244(6) 0.9549(6) 0.0403(16) Uani 1 1 d . . . O4 O -0.2413(8) 0.1826(8) 0.7660(7) 0.062(2) Uani 1 1 d . . . O5 O 0.3140(13) 0.5231(14) 0.8619(11) 0.115(4) Uani 1 1 d . . . H5 H 0.3383 0.4708 0.8145 0.173 Uiso 1 1 calc R . . O6 O -0.3431(10) 0.3233(9) 0.5514(8) 0.087(3) Uani 1 1 d . . . O7 O 0.3317(10) 0.4515(8) 0.6492(7) 0.069(2) Uani 1 1 d . . . N1 N 0.0199(9) 0.2287(8) 1.1699(8) 0.043(2) Uani 1 1 d . . . N2 N 0.0784(9) 0.3249(8) 1.0803(8) 0.043(2) Uani 1 1 d . . . N3 N -0.0004(8) 0.2314(7) 0.9897(7) 0.0344(18) Uani 1 1 d . . . N4 N 0.2168(8) 0.3469(8) 1.2716(7) 0.0370(19) Uani 1 1 d . . . N5 N 0.1711(10) 0.3808(9) 1.3885(8) 0.057(2) Uani 1 1 d . . . N6 N 0.1480(8) 0.5765(8) 1.2276(7) 0.0389(19) Uani 1 1 d . . . C1 C 0.0036(12) 0.2102(11) 1.3054(9) 0.046(3) Uani 1 1 d . . . H1A H -0.0635 0.1580 1.3592 0.055 Uiso 1 1 calc R . . H1B H -0.0449 0.3022 1.3271 0.055 Uiso 1 1 calc R . . C2 C 0.1516(12) 0.1342(10) 1.3386(11) 0.054(3) Uani 1 1 d . . . H2A H 0.1290 0.1276 1.4303 0.065 Uiso 1 1 calc R . . H2B H 0.1950 0.0390 1.3248 0.065 Uiso 1 1 calc R . . C3 C 0.2689(11) 0.2018(9) 1.2622(10) 0.048(3) Uani 1 1 d . . . H3A H 0.3575 0.1471 1.2925 0.057 Uiso 1 1 calc R . . H3B H 0.3005 0.1986 1.1715 0.057 Uiso 1 1 calc R . . C4 C 0.0687(10) 0.3221(9) 0.9748(8) 0.032(2) Uani 1 1 d . . . H4A H 0.1047 0.3762 0.8947 0.039 Uiso 1 1 calc R . . C5 C -0.0314(10) 0.1789(9) 1.1193(8) 0.029(2) Uani 1 1 d . . . H5A H -0.0823 0.1160 1.1655 0.035 Uiso 1 1 calc R . . C6 C 0.1346(13) 0.5206(11) 1.3522(10) 0.053(3) Uani 1 1 d . . . H6A H 0.1016 0.5755 1.4116 0.064 Uiso 1 1 calc R . . C7 C 0.2006(10) 0.4644(9) 1.1769(9) 0.036(2) Uani 1 1 d . . . H7A H 0.2226 0.4670 1.0897 0.043 Uiso 1 1 calc R . . C8 C 0.3652(10) 0.0771(10) 0.5812(8) 0.035(2) Uani 1 1 d . . . C9 C 0.4815(10) 0.1256(9) 0.5200(8) 0.036(2) Uani 1 1 d . . . H9A H 0.4719 0.2088 0.5332 0.043 Uiso 1 1 calc R . . C10 C 0.6172(11) 0.0493(10) 0.4363(10) 0.046(3) Uani 1 1 d . . . H10A H 0.6959 0.0840 0.3924 0.055 Uiso 1 1 calc R . . C11 C 0.2191(10) 0.1536(9) 0.6755(9) 0.035(2) Uani 1 1 d . . . C12 C -0.3931(10) 0.0653(9) 0.9478(9) 0.038(2) Uani 1 1 d . . . C13 C -0.4000(10) -0.0288(9) 1.0649(9) 0.035(2) Uani 1 1 d . . . H13A H -0.3315 -0.0502 1.1077 0.042 Uiso 1 1 calc R . . C14 C -0.5075(10) -0.0928(10) 1.1208(9) 0.041(2) Uani 1 1 d . . . H14A H -0.5144 -0.1529 1.2023 0.049 Uiso 1 1 calc R . . C15 C -0.2741(10) 0.1334(9) 0.8842(10) 0.035(2) Uani 1 1 d . . . C16 C 0.4338(17) 0.568(2) 0.831(2) 0.164(10) Uani 1 1 d . . . H16A H 0.3933 0.6669 0.8303 0.246 Uiso 1 1 calc R . . H16B H 0.5024 0.5526 0.7460 0.246 Uiso 1 1 calc R . . H16C H 0.4874 0.5162 0.8938 0.246 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0295(7) 0.0350(7) 0.0452(8) -0.0127(5) -0.0065(5) -0.0147(5) O1 0.028(4) 0.043(4) 0.038(4) -0.006(3) 0.003(3) -0.022(3) O2 0.038(4) 0.049(4) 0.061(5) -0.027(4) 0.001(4) -0.016(3) O3 0.044(4) 0.041(4) 0.044(4) 0.001(3) -0.016(3) -0.027(3) O4 0.055(5) 0.072(5) 0.061(5) 0.006(4) -0.011(4) -0.046(4) O5 0.096(8) 0.150(11) 0.104(8) -0.055(7) 0.014(7) -0.066(8) O6 0.085(7) 0.094(7) 0.061(5) 0.026(4) -0.022(5) -0.048(5) O7 0.089(6) 0.072(5) 0.058(5) -0.011(4) -0.012(5) -0.050(5) N1 0.040(5) 0.036(5) 0.053(5) -0.006(4) -0.015(4) -0.016(4) N2 0.051(5) 0.041(5) 0.050(5) 0.006(4) -0.024(4) -0.030(4) N3 0.031(4) 0.034(4) 0.042(5) -0.009(3) -0.012(4) -0.012(3) N4 0.043(5) 0.038(4) 0.028(4) -0.011(4) -0.016(4) -0.006(4) N5 0.066(6) 0.041(5) 0.059(6) -0.018(4) -0.016(5) -0.013(4) N6 0.036(5) 0.042(5) 0.033(4) -0.008(4) -0.001(4) -0.017(4) C1 0.055(7) 0.067(7) 0.026(5) -0.003(5) -0.010(5) -0.039(6) C2 0.063(7) 0.027(5) 0.063(7) 0.006(5) -0.021(6) -0.020(5) C3 0.050(7) 0.038(6) 0.053(6) -0.014(5) -0.027(6) -0.002(5) C4 0.044(6) 0.040(5) 0.021(4) -0.006(4) -0.005(4) -0.025(4) C5 0.035(5) 0.038(5) 0.022(4) -0.005(4) -0.004(4) -0.023(4) C6 0.067(8) 0.057(7) 0.039(6) -0.025(5) -0.009(6) -0.020(6) C7 0.031(5) 0.034(5) 0.036(5) -0.011(4) -0.007(4) -0.008(4) C8 0.029(5) 0.051(6) 0.025(5) -0.015(4) -0.010(4) -0.006(4) C9 0.030(5) 0.033(5) 0.038(5) -0.020(4) 0.009(5) -0.015(4) C10 0.038(6) 0.043(6) 0.062(7) -0.018(5) -0.008(6) -0.019(5) C11 0.033(6) 0.027(5) 0.041(5) -0.003(4) -0.013(5) -0.009(4) C12 0.027(5) 0.032(5) 0.053(6) -0.007(5) -0.012(5) -0.009(4) C13 0.036(6) 0.030(5) 0.041(5) -0.007(4) -0.014(5) -0.013(4) C14 0.036(6) 0.050(6) 0.048(6) 0.006(5) -0.024(5) -0.026(5) C15 0.031(5) 0.029(5) 0.044(6) -0.014(4) -0.005(5) -0.010(4) C16 0.052(11) 0.19(2) 0.29(3) -0.13(2) -0.015(14) -0.046(12) _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 O3 1.951(6) . ? Zn1 O1 1.962(6) . ? Zn1 N6 2.006(7) 2_567 ? Zn1 N3 2.010(7) . ? O1 C11 1.267(10) . ? O2 C11 1.251(10) . ? O3 C15 1.254(11) . ? O4 C15 1.235(10) . ? O5 C16 1.404(17) . ? O5 H5 0.8200 . ? N1 C5 1.298(11) . ? N1 N2 1.348(10) . ? N1 C1 1.454(12) . ? N2 C4 1.280(11) . ? N3 C5 1.353(10) . ? N3 C4 1.395(11) . ? N4 C7 1.349(11) . ? N4 N5 1.365(10) . ? N4 C3 1.452(11) . ? N5 C6 1.338(12) . ? N6 C6 1.323(11) . ? N6 C7 1.335(11) . ? N6 Zn1 2.006(7) 2_567 ? C1 C2 1.514(14) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.503(13) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.355(12) . ? C8 C10 1.386(13) 2_656 ? C8 C11 1.518(13) . ? C9 C10 1.409(12) . ? C9 H9A 0.9300 . ? C10 C8 1.386(13) 2_656 ? C10 H10A 0.9300 . ? C12 C13 1.371(12) . ? C12 C14 1.420(12) 2_457 ? C12 C15 1.518(12) . ? C13 C14 1.390(12) . ? C13 H13A 0.9300 . ? C14 C12 1.420(12) 2_457 ? C14 H14A 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? 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 O3 Zn1 O1 110.1(3) . . ? O3 Zn1 N6 115.6(3) . 2_567 ? O1 Zn1 N6 115.1(3) . 2_567 ? O3 Zn1 N3 101.0(3) . . ? O1 Zn1 N3 113.0(3) . . ? N6 Zn1 N3 100.7(3) 2_567 . ? C11 O1 Zn1 110.6(6) . . ? C15 O3 Zn1 108.4(6) . . ? C16 O5 H5 109.5 . . ? C5 N1 N2 111.1(8) . . ? C5 N1 C1 129.7(8) . . ? N2 N1 C1 118.6(8) . . ? C4 N2 N1 103.4(7) . . ? C5 N3 C4 100.5(7) . . ? C5 N3 Zn1 133.5(6) . . ? C4 N3 Zn1 125.3(6) . . ? C7 N4 N5 110.2(7) . . ? C7 N4 C3 128.9(8) . . ? N5 N4 C3 120.9(7) . . ? C6 N5 N4 100.7(8) . . ? C6 N6 C7 103.0(8) . . ? C6 N6 Zn1 126.2(7) . 2_567 ? C7 N6 Zn1 129.0(6) . 2_567 ? N1 C1 C2 114.7(9) . . ? N1 C1 H1A 108.6 . . ? C2 C1 H1A 108.6 . . ? N1 C1 H1B 108.6 . . ? C2 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? C3 C2 C1 115.1(8) . . ? C3 C2 H2A 108.5 . . ? C1 C2 H2A 108.5 . . ? C3 C2 H2B 108.5 . . ? C1 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? N4 C3 C2 114.2(8) . . ? N4 C3 H3A 108.7 . . ? C2 C3 H3A 108.7 . . ? N4 C3 H3B 108.7 . . ? C2 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? N2 C4 N3 114.6(8) . . ? N2 C4 H4A 122.7 . . ? N3 C4 H4A 122.7 . . ? N1 C5 N3 110.2(8) . . ? N1 C5 H5A 124.9 . . ? N3 C5 H5A 124.9 . . ? N6 C6 N5 116.6(9) . . ? N6 C6 H6A 121.7 . . ? N5 C6 H6A 121.7 . . ? N6 C7 N4 109.4(8) . . ? N6 C7 H7A 125.3 . . ? N4 C7 H7A 125.3 . . ? C9 C8 C10 119.6(8) . 2_656 ? C9 C8 C11 121.3(8) . . ? C10 C8 C11 119.0(8) 2_656 . ? C8 C9 C10 119.6(8) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? C8 C10 C9 120.7(9) 2_656 . ? C8 C10 H10A 119.6 2_656 . ? C9 C10 H10A 119.6 . . ? O2 C11 O1 123.0(8) . . ? O2 C11 C8 118.2(8) . . ? O1 C11 C8 118.9(8) . . ? C13 C12 C14 119.5(8) . 2_457 ? C13 C12 C15 121.8(8) . . ? C14 C12 C15 118.6(8) 2_457 . ? C12 C13 C14 121.2(9) . . ? C12 C13 H13A 119.4 . . ? C14 C13 H13A 119.4 . . ? C13 C14 C12 119.2(8) . 2_457 ? C13 C14 H14A 120.4 . . ? C12 C14 H14A 120.4 2_457 . ? O4 C15 O3 123.7(9) . . ? O4 C15 C12 119.5(9) . . ? O3 C15 C12 116.5(8) . . ? O5 C16 H16A 109.5 . . ? O5 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O5 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Zn1 O1 C11 -169.9(5) . . . . ? N6 Zn1 O1 C11 57.2(6) 2_567 . . . ? N3 Zn1 O1 C11 -57.7(6) . . . . ? O1 Zn1 O3 C15 -73.1(6) . . . . ? N6 Zn1 O3 C15 59.5(6) 2_567 . . . ? N3 Zn1 O3 C15 167.1(6) . . . . ? C5 N1 N2 C4 -4.2(10) . . . . ? C1 N1 N2 C4 -176.0(8) . . . . ? O3 Zn1 N3 C5 7.3(8) . . . . ? O1 Zn1 N3 C5 -110.4(8) . . . . ? N6 Zn1 N3 C5 126.3(8) 2_567 . . . ? O3 Zn1 N3 C4 -161.5(7) . . . . ? O1 Zn1 N3 C4 80.8(7) . . . . ? N6 Zn1 N3 C4 -42.5(7) 2_567 . . . ? C7 N4 N5 C6 -2.0(11) . . . . ? C3 N4 N5 C6 179.8(9) . . . . ? C5 N1 C1 C2 116.4(10) . . . . ? N2 N1 C1 C2 -73.5(11) . . . . ? N1 C1 C2 C3 57.9(12) . . . . ? C7 N4 C3 C2 -116.8(10) . . . . ? N5 N4 C3 C2 61.0(12) . . . . ? C1 C2 C3 N4 56.7(12) . . . . ? N1 N2 C4 N3 2.5(10) . . . . ? C5 N3 C4 N2 -0.1(10) . . . . ? Zn1 N3 C4 N2 171.7(6) . . . . ? N2 N1 C5 N3 4.4(11) . . . . ? C1 N1 C5 N3 175.1(9) . . . . ? C4 N3 C5 N1 -2.6(9) . . . . ? Zn1 N3 C5 N1 -173.3(6) . . . . ? C7 N6 C6 N5 -1.3(12) . . . . ? Zn1 N6 C6 N5 164.8(7) 2_567 . . . ? N4 N5 C6 N6 2.1(12) . . . . ? C6 N6 C7 N4 -0.1(10) . . . . ? Zn1 N6 C7 N4 -165.7(6) 2_567 . . . ? N5 N4 C7 N6 1.4(10) . . . . ? C3 N4 C7 N6 179.4(8) . . . . ? C10 C8 C9 C10 1.9(15) 2_656 . . . ? C11 C8 C9 C10 178.0(8) . . . . ? C8 C9 C10 C8 -1.9(15) . . . 2_656 ? Zn1 O1 C11 O2 -1.5(11) . . . . ? Zn1 O1 C11 C8 177.9(6) . . . . ? C9 C8 C11 O2 -1.3(13) . . . . ? C10 C8 C11 O2 174.8(8) 2_656 . . . ? C9 C8 C11 O1 179.3(8) . . . . ? C10 C8 C11 O1 -4.6(12) 2_656 . . . ? C14 C12 C13 C14 -3.2(15) 2_457 . . . ? C15 C12 C13 C14 -178.6(8) . . . . ? C12 C13 C14 C12 3.2(15) . . . 2_457 ? Zn1 O3 C15 O4 6.4(11) . . . . ? Zn1 O3 C15 C12 179.8(6) . . . . ? C13 C12 C15 O4 158.6(9) . . . . ? C14 C12 C15 O4 -16.9(13) 2_457 . . . ? C13 C12 C15 O3 -15.1(13) . . . . ? C14 C12 C15 O3 169.5(8) 2_457 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 O7 0.82 2.03 2.759(14) 147.2 . _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.838 _refine_diff_density_min -0.893 _refine_diff_density_rms 0.207 ###======