# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge ? _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jian Zhang' _publ_contact_author_email zhj@fjirsm.ac.cn loop_ _publ_author_name 'Jian Zhang' 'Hui Yang' 'Hai-Xia Zhang' 'Duan-Chuan Hou' 'Tie-Hu Li' data_1 _database_code_depnum_ccdc_archive 'CCDC 868806' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 N6 O14 Zn3' _chemical_formula_sum 'C24 H24 N6 O14 Zn3' _chemical_formula_weight 816.657 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 Hexagonal _symmetry_space_group_name_H-M P6(3)cm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' _cell_length_a 18.5924(8) _cell_length_b 18.5924(8) _cell_length_c 17.9643(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5377.9(4) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1790 _cell_measurement_theta_min 2.4619 _cell_measurement_theta_max 29.1146 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2358 _exptl_absorpt_coefficient_mu 2.056 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.5330 _exptl_absorpt_correction_T_max 0.5967 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The contribution of the disordered atoms were subtracted from the reflection data by the SQUEEZE method Because of the free guest molecules are unknown in the compound, so the correct and complete framework formular should be [Zn9(¦Ì3-OH)3(btc)5(e-urea)9](solvent)x ; _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 10873 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3141 _reflns_number_gt 2492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SMART and SAINT (Siemens,1994)' _computing_data_reduction 'SMART and SAINT (Siemens,1994)' _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1137P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_number_reflns 3141 _refine_ls_number_parameters 229 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.1870 _refine_ls_wR_factor_gt 0.1766 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.079 _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 Zn1 Zn 0.90074(6) 0.24296(6) 0.38071(5) 0.0353(3) Uani 1 1 d . . . Zn2 Zn 0.65581(7) 0.0000 0.72332(9) 0.0456(4) Uani 1 2 d S . . O1 O 0.7925(4) 0.2365(4) 0.3907(5) 0.061(2) Uani 1 1 d . . . O2 O 0.8756(5) 0.3610(6) 0.4254(5) 0.076(2) Uani 1 1 d . . . O3 O 0.7798(5) 0.0902(6) 0.7103(4) 0.075(3) Uani 1 1 d . . . O4 O 0.8489(4) 0.1224(5) 0.8156(3) 0.0504(18) Uani 1 1 d . . . O5 O 0.9316(4) 0.2181(4) 0.4790(3) 0.0464(16) Uani 1 1 d . . . O6 O 1.0000 0.3396(4) 0.3382(4) 0.0297(19) Uani 1 2 d S . . O7 O 0.6325(7) 0.0000 0.6130(7) 0.088(4) Uani 1 2 d S . . O8 O 0.6215(7) 0.0920(7) 0.7378(5) 0.095(3) Uani 1 1 d . . . C1 C 0.8082(6) 0.3070(7) 0.4113(6) 0.046(2) Uani 1 1 d . . . C2 C 0.7329(7) 0.3197(7) 0.4136(7) 0.053(3) Uani 1 1 d . . . C3 C 0.7460(6) 0.4002(6) 0.4148(6) 0.046(2) Uani 1 1 d . . . H3A H 0.7998 0.4452 0.4163 0.055 Uiso 1 1 calc R . . C4 C 0.8442(6) 0.1221(6) 0.7457(4) 0.037(2) Uani 1 1 d . . . C5 C 0.9260(5) 0.1683(5) 0.7051(4) 0.035(2) Uani 1 1 d . . . C6 C 0.9253(5) 0.1859(6) 0.6277(5) 0.036(2) Uani 1 1 d . . . H6A H 0.8756 0.1696 0.6028 0.043 Uiso 1 1 calc R . . C7 C 1.0000 0.2276(6) 0.5912(6) 0.030(3) Uani 1 2 d S . . C8 C 1.0000 0.2468(7) 0.5083(6) 0.031(3) Uani 1 2 d S . . C9 C 1.0000 0.2009(6) 0.7430(6) 0.036(3) Uani 1 2 d S . . H9A H 1.0000 0.1949 0.7944 0.043 Uiso 1 2 calc SR . . C10 C 0.6781(13) 0.0000 0.5553(13) 0.099(3) Uani 1 2 d SU . . C11 C 0.7092(13) 0.0000 0.4300(11) 0.100(3) Uani 1 2 d SU . . C12 C 0.7755(13) 0.0000 0.4782(12) 0.100(3) Uani 1 2 d SU . . C13 C 0.578(2) 0.114(2) 0.7088(17) 0.256(6) Uani 1 1 d U . . C14 C 0.518(3) 0.167(3) 0.6243(18) 0.263(6) Uani 1 1 d U . . C15 C 0.489(3) 0.167(3) 0.6992(19) 0.261(6) Uani 1 1 d U . . N1 N 0.6484(11) 0.0000 0.4875(10) 0.100(3) Uani 1 2 d SU . . N2 N 0.7478(10) 0.0000 0.5566(9) 0.099(3) Uani 1 2 d SU . . N3 N 0.5482(19) 0.1013(18) 0.6461(12) 0.256(6) Uani 1 1 d U . . N4 N 0.5245(18) 0.138(2) 0.7416(12) 0.259(6) Uani 1 1 d U . . 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 0.0400(5) 0.0479(6) 0.0200(4) -0.0030(6) -0.0037(5) 0.0234(4) Zn2 0.0456(6) 0.0768(12) 0.0247(7) 0.000 -0.0034(6) 0.0384(6) O1 0.062(4) 0.059(4) 0.080(6) 0.000(4) 0.003(5) 0.044(4) O2 0.046(5) 0.086(6) 0.095(6) -0.023(5) 0.001(4) 0.031(5) O3 0.045(4) 0.128(8) 0.029(4) 0.006(4) 0.001(3) 0.027(5) O4 0.059(4) 0.083(5) 0.024(3) 0.009(3) 0.011(3) 0.046(4) O5 0.043(4) 0.065(4) 0.019(3) 0.007(3) -0.003(3) 0.018(4) O6 0.049(5) 0.030(3) 0.016(4) 0.004(3) 0.000 0.024(3) O7 0.094(6) 0.119(11) 0.058(8) 0.000 -0.016(6) 0.060(6) O8 0.124(8) 0.134(8) 0.072(7) 0.013(6) 0.013(6) 0.098(7) C1 0.040(6) 0.052(6) 0.044(5) -0.005(5) 0.001(4) 0.022(5) C2 0.051(6) 0.055(7) 0.058(6) -0.003(5) 0.003(5) 0.031(6) C3 0.039(5) 0.047(6) 0.052(6) -0.008(5) -0.006(4) 0.023(5) C4 0.044(5) 0.053(5) 0.022(4) -0.003(4) -0.003(4) 0.031(5) C5 0.040(5) 0.046(5) 0.015(4) 0.007(4) 0.008(4) 0.018(4) C6 0.031(4) 0.060(6) 0.023(4) -0.004(4) -0.001(4) 0.027(4) C7 0.032(6) 0.037(5) 0.018(5) 0.000(4) 0.000 0.016(3) C8 0.035(7) 0.040(5) 0.017(5) -0.001(4) 0.000 0.017(4) C9 0.067(9) 0.033(4) 0.019(6) 0.004(4) 0.000 0.033(4) C10 0.107(5) 0.140(8) 0.062(6) 0.000 0.009(4) 0.070(4) C11 0.107(5) 0.140(8) 0.064(6) 0.000 0.010(4) 0.070(4) C12 0.107(5) 0.140(8) 0.063(6) 0.000 0.010(4) 0.070(4) C13 0.384(15) 0.449(16) 0.150(9) -0.067(12) -0.083(11) 0.370(14) C14 0.388(16) 0.453(16) 0.153(10) -0.067(12) -0.082(11) 0.363(14) C15 0.386(16) 0.452(16) 0.152(10) -0.067(12) -0.082(11) 0.365(14) N1 0.108(5) 0.140(8) 0.063(6) 0.000 0.009(4) 0.070(4) N2 0.107(5) 0.140(8) 0.062(6) 0.000 0.010(4) 0.070(4) N3 0.385(15) 0.449(16) 0.150(10) -0.067(12) -0.084(11) 0.370(14) N4 0.385(15) 0.451(16) 0.152(9) -0.067(12) -0.082(11) 0.368(14) _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 O4 1.933(6) 7_664 ? Zn1 O1 1.964(6) . ? Zn1 O6 1.975(4) . ? Zn1 O5 1.980(6) . ? Zn2 O7 2.028(12) . ? Zn2 O6 2.066(8) 6_545 ? Zn2 O3 2.078(8) 11 ? Zn2 O3 2.078(8) . ? Zn2 O8 2.120(9) 11 ? Zn2 O8 2.120(9) . ? O1 C1 1.247(12) . ? O2 C1 1.176(12) . ? O3 C4 1.217(11) . ? O4 C4 1.259(10) . ? O4 Zn1 1.933(6) 7_665 ? O5 C8 1.226(7) . ? O6 Zn1 1.975(4) 12_765 ? O6 Zn2 2.066(8) 5_664 ? O7 C10 1.34(2) . ? O8 C13 1.21(2) . ? C1 C2 1.533(15) . ? C2 C3 1.359(13) 3_665 ? C2 C3 1.392(13) . ? C3 C2 1.359(13) 2_655 ? C3 H3A 0.9300 . ? C4 C5 1.508(12) . ? C5 C9 1.375(10) . ? C5 C6 1.430(11) . ? C6 C7 1.372(10) . ? C6 H6A 0.9300 . ? C7 C6 1.372(10) 12_765 ? C7 C8 1.532(14) . ? C8 O5 1.226(7) 12_765 ? C9 C5 1.375(10) 12_765 ? C9 H9A 0.9300 . ? C10 N2 1.30(3) . ? C10 N1 1.34(3) . ? C11 C12 1.51(3) . ? C11 N1 1.53(3) . ? C12 N2 1.50(2) . ? C13 N3 1.22(3) . ? C13 N4 1.39(3) . ? C14 C15 1.45(4) . ? C14 N3 1.64(3) . ? C15 N4 1.29(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 O4 Zn1 O1 103.4(3) 7_664 . ? O4 Zn1 O6 105.3(3) 7_664 . ? O1 Zn1 O6 123.6(3) . . ? O4 Zn1 O5 107.2(3) 7_664 . ? O1 Zn1 O5 108.2(3) . . ? O6 Zn1 O5 108.0(3) . . ? O7 Zn2 O6 170.0(5) . 6_545 ? O7 Zn2 O3 92.3(4) . 11 ? O6 Zn2 O3 94.8(3) 6_545 11 ? O7 Zn2 O3 92.3(4) . . ? O6 Zn2 O3 94.8(3) 6_545 . ? O3 Zn2 O3 88.7(6) 11 . ? O7 Zn2 O8 88.2(4) . 11 ? O6 Zn2 O8 84.6(3) 6_545 11 ? O3 Zn2 O8 91.3(4) 11 11 ? O3 Zn2 O8 179.4(3) . 11 ? O7 Zn2 O8 88.2(4) . . ? O6 Zn2 O8 84.6(3) 6_545 . ? O3 Zn2 O8 179.4(3) 11 . ? O3 Zn2 O8 91.3(4) . . ? O8 Zn2 O8 88.7(6) 11 . ? C1 O1 Zn1 105.5(6) . . ? C4 O3 Zn2 139.4(7) . . ? C4 O4 Zn1 123.5(6) . 7_665 ? C8 O5 Zn1 129.8(6) . . ? Zn1 O6 Zn1 108.0(3) 12_765 . ? Zn1 O6 Zn2 113.9(3) 12_765 5_664 ? Zn1 O6 Zn2 113.9(3) . 5_664 ? C10 O7 Zn2 128.4(14) . . ? C13 O8 Zn2 139.1(17) . . ? O2 C1 O1 123.5(10) . . ? O2 C1 C2 121.8(11) . . ? O1 C1 C2 114.7(9) . . ? C3 C2 C3 119.8(11) 3_665 . ? C3 C2 C1 121.2(10) 3_665 . ? C3 C2 C1 119.0(10) . . ? C2 C3 C2 120.1(11) 2_655 . ? C2 C3 H3A 119.9 2_655 . ? C2 C3 H3A 119.9 . . ? O3 C4 O4 125.0(9) . . ? O3 C4 C5 119.4(7) . . ? O4 C4 C5 115.6(8) . . ? C9 C5 C6 120.1(8) . . ? C9 C5 C4 120.9(7) . . ? C6 C5 C4 118.6(8) . . ? C7 C6 C5 118.1(8) . . ? C7 C6 H6A 120.9 . . ? C5 C6 H6A 120.9 . . ? C6 C7 C6 122.5(10) 12_765 . ? C6 C7 C8 118.6(5) 12_765 . ? C6 C7 C8 118.6(5) . . ? O5 C8 O5 128.1(10) . 12_765 ? O5 C8 C7 115.9(5) . . ? O5 C8 C7 115.9(5) 12_765 . ? C5 C9 C5 120.2(10) . 12_765 ? C5 C9 H9A 119.9 . . ? C5 C9 H9A 119.9 12_765 . ? N2 C10 O7 128(2) . . ? N2 C10 N1 115(2) . . ? O7 C10 N1 116(2) . . ? C12 C11 N1 102.4(17) . . ? C11 C12 N2 105.0(18) . . ? O8 C13 N3 130(3) . . ? O8 C13 N4 129(3) . . ? N3 C13 N4 98(2) . . ? C15 C14 N3 92(2) . . ? N4 C15 C14 107(3) . . ? C10 N1 C11 108.1(19) . . ? C10 N2 C12 109.1(18) . . ? C13 N3 C14 111(2) . . ? C15 N4 C13 118(3) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.001 470.3 81.2 2 0.000 0.569 0.057 26.4 10.3 3 0.569 0.000 0.057 26.4 10.5 4 0.431 0.431 0.057 26.7 11.1 5 0.182 0.452 0.046 16.6 3.0 6 0.270 0.818 0.046 16.6 3.1 7 0.452 0.182 0.046 16.5 3.0 8 0.548 0.730 0.046 16.5 3.1 9 0.730 0.548 0.046 16.5 3.3 10 0.818 0.270 0.046 16.5 3.0 11 0.333 0.667 0.065 7.4 -0.3 12 0.667 0.333 0.065 7.4 -0.4 13 0.333 0.667 0.229 21.2 1.0 14 0.667 0.333 0.229 21.2 0.8 15 0.000 0.585 0.322 46.3 35.7 16 0.415 0.415 0.322 45.8 36.6 17 0.585 0.000 0.322 46.3 36.2 18 0.000 0.430 0.558 26.4 11.0 19 0.430 0.000 0.558 26.3 10.6 20 0.570 0.570 0.558 26.2 10.1 21 0.182 0.730 0.546 16.6 3.4 22 0.270 0.452 0.546 16.5 3.3 23 0.452 0.270 0.546 16.5 3.4 24 0.547 0.818 0.546 16.5 3.4 25 0.730 0.182 0.546 16.5 3.3 26 0.818 0.548 0.546 16.5 3.6 27 0.333 0.667 0.565 7.4 -0.7 28 0.667 0.333 0.565 7.4 -0.7 29 0.333 0.667 0.729 21.2 -0.3 30 0.667 0.333 0.729 21.2 -0.4 31 0.000 0.414 0.821 45.8 38.4 32 0.414 0.000 0.821 45.9 37.8 33 0.586 0.586 0.821 45.9 37.5 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.555 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.201 #end data_2 _database_code_depnum_ccdc_archive 'CCDC 868809' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H31 N3 O22 Zn5' _chemical_formula_sum 'C39 H31 N3 O22 Zn5' _chemical_formula_weight 1220.63 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 18.060(12) _cell_length_b 12.104(8) _cell_length_c 31.65(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.480(15) _cell_angle_gamma 90.00 _cell_volume 6919(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2444 _exptl_absorpt_coefficient_mu 1.766 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6194 _exptl_absorpt_correction_T_max 0.7190 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The contribution of the disordered atoms were subtracted from the reflection data by the SQUEEZE method The main reason of high R factor may be due to the disordered atoms Because of the free guest molecules are unknown in the compound, so the correct and complete framework formular should be [Zn5(¦Ì3-OH)(btc)3(pyrol)3](solvent)x ; _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 37870 _diffrn_reflns_av_R_equivalents 0.1116 _diffrn_reflns_av_sigmaI/netI 0.1536 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11972 _reflns_number_gt 7056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SMART and SAINT (Siemens,1994)' _computing_data_reduction 'SMART and SAINT (Siemens,1994)' _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 11972 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1403 _refine_ls_R_factor_gt 0.1136 _refine_ls_wR_factor_ref 0.3191 _refine_ls_wR_factor_gt 0.2915 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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 0.04406(6) 0.59888(11) 0.51347(4) 0.0422(4) Uani 1 1 d . . . Zn2 Zn 0.54498(5) 0.40093(8) 0.48757(3) 0.0199(3) Uani 1 1 d . . . Zn3 Zn 0.66586(6) 0.50203(8) 0.19005(3) 0.0242(3) Uani 1 1 d . . . Zn4 Zn 0.75465(6) 0.40818(8) 0.26871(3) 0.0269(3) Uani 1 1 d . . . Zn5 Zn 0.85463(7) 0.53162(12) 0.19460(4) 0.0476(4) Uani 1 1 d . . . O1 O 0.0914(6) 0.9187(11) 0.3430(4) 0.103(5) Uani 1 1 d . . . O2 O 0.0598(6) 0.8844(9) 0.2779(4) 0.089(3) Uani 1 1 d . . . O3 O -0.1532(8) 0.6126(8) 0.2514(4) 0.111(5) Uani 1 1 d . . . O4 O -0.1662(5) 0.4860(8) 0.3012(3) 0.058(2) Uani 1 1 d . . . O5 O -0.0458(6) 0.5105(9) 0.4364(3) 0.074(3) Uani 1 1 d . . . O6 O 0.0194(5) 0.6558(8) 0.4553(3) 0.061(2) Uani 1 1 d . . . O7 O 0.3993(6) 0.8252(8) 0.2716(2) 0.081(3) Uani 1 1 d . . . O8 O 0.3991(4) 0.8921(5) 0.3366(2) 0.0381(17) Uani 1 1 d . . . O9 O 0.4838(4) 0.6273(6) 0.45015(19) 0.0420(18) Uani 1 1 d . . . O10 O 0.5524(4) 0.4783(6) 0.4303(2) 0.0444(18) Uani 1 1 d . . . O11 O 0.6678(4) 0.4805(6) 0.29321(19) 0.0361(16) Uani 1 1 d . . . O12 O 0.6204(4) 0.5797(5) 0.23915(17) 0.0305(14) Uani 1 1 d . . . O13 O 0.1125(4) 0.4826(7) 0.4845(3) 0.054(2) Uani 1 1 d . . . O14 O 0.0484(4) 0.3308(8) 0.4619(3) 0.060(2) Uani 1 1 d . . . O15 O 0.1946(4) 0.1167(7) 0.3528(3) 0.056(2) Uani 1 1 d . . . O16 O 0.3170(4) 0.1143(6) 0.3546(2) 0.0375(17) Uani 1 1 d . . . O17 O 0.4455(3) 0.3437(6) 0.4682(2) 0.0377(16) Uani 1 1 d . . . O18 O 0.3796(4) 0.4910(6) 0.4894(2) 0.0375(16) Uani 1 1 d . . . O19 O 0.1187(4) 0.7105(6) 0.5313(2) 0.0480(19) Uani 1 1 d . . . O20 O 0.6045(4) 0.2622(5) 0.47885(19) 0.0342(15) Uani 1 1 d . . . O21 O 0.7595(4) 0.2559(6) 0.2878(2) 0.0497(19) Uani 1 1 d . . . O22 O 0.7612(4) 0.4356(5) 0.20845(18) 0.0310(14) Uani 1 1 d . . . C1 C 0.0076(7) 0.7746(11) 0.3297(4) 0.058(3) Uani 1 1 d . . . C2 C -0.0413(7) 0.7202(10) 0.3011(4) 0.053(3) Uani 1 1 d . . . H3 H -0.0434 0.7430 0.2724 0.063 Uiso 1 1 calc R . . C3 C -0.0873(7) 0.6319(10) 0.3151(4) 0.050(3) Uani 1 1 d . . . C4 C -0.0818(8) 0.5959(11) 0.3568(4) 0.063(4) Uani 1 1 d . . . H6 H -0.1126 0.5379 0.3666 0.075 Uiso 1 1 calc R . . C5 C -0.0283(6) 0.6484(11) 0.3853(4) 0.049(3) Uani 1 1 d . . . C6 C 0.0160(6) 0.7371(11) 0.3723(4) 0.057(3) Uani 1 1 d . . . H9 H 0.0504 0.7711 0.3912 0.069 Uiso 1 1 calc R . . C7 C 0.0541(7) 0.8659(14) 0.3156(5) 0.070(4) Uani 1 1 d . . . C8 C -0.1362(7) 0.5755(10) 0.2875(4) 0.054(3) Uani 1 1 d . . . C9 C -0.0199(7) 0.6035(11) 0.4293(4) 0.054(3) Uani 1 1 d . . . C10 C 0.4713(7) 0.7317(9) 0.3239(3) 0.045(3) Uani 1 1 d . . . C11 C 0.4719(6) 0.6967(8) 0.3650(3) 0.039(2) Uani 1 1 d . . . H12 H 0.4400 0.7304 0.3849 0.046 Uiso 1 1 calc R . . C12 C 0.5205(6) 0.6092(8) 0.3781(3) 0.036(2) Uani 1 1 d . . . C13 C 0.5673(5) 0.5651(8) 0.3499(2) 0.032(2) Uani 1 1 d . . . H15 H 0.5999 0.5078 0.3588 0.038 Uiso 1 1 calc R . . C14 C 0.5697(5) 0.6011(7) 0.3071(3) 0.028(2) Uani 1 1 d . . . C15 C 0.5203(6) 0.6823(9) 0.2937(3) 0.037(2) Uani 1 1 d . . . H18 H 0.5190 0.7048 0.2650 0.045 Uiso 1 1 calc R . . C16 C 0.4193(5) 0.8245(9) 0.3093(3) 0.038(2) Uani 1 1 d . . . C17 C 0.5182(6) 0.5661(9) 0.4231(3) 0.037(2) Uani 1 1 d . . . C18 C 0.6221(5) 0.5483(7) 0.2775(3) 0.027(2) Uani 1 1 d . . . C19 C 0.1820(6) 0.3447(11) 0.4511(3) 0.049(3) Uani 1 1 d . . . C20 C 0.1846(6) 0.2579(10) 0.4185(3) 0.046(3) Uani 1 1 d . . . H21 H 0.1409 0.2218 0.4090 0.055 Uiso 1 1 calc R . . C21 C 0.2505(5) 0.2320(8) 0.4029(3) 0.030(2) Uani 1 1 d . . . C22 C 0.3214(5) 0.2676(7) 0.4214(3) 0.0268(19) Uani 1 1 d . . . H24 H 0.3676 0.2386 0.4126 0.032 Uiso 1 1 calc R . . C23 C 0.3154(5) 0.3492(8) 0.4537(3) 0.033(2) Uani 1 1 d . . . C24 C 0.2467(5) 0.3873(9) 0.4668(3) 0.036(2) Uani 1 1 d . . . H27 H 0.2446 0.4446 0.4873 0.044 Uiso 1 1 calc R . . C25 C 0.1102(7) 0.3867(11) 0.4662(4) 0.052(3) Uani 1 1 d . . . C26 C 0.2543(5) 0.1461(8) 0.3675(3) 0.0256(19) Uani 1 1 d . . . C27 C 0.3830(5) 0.3975(8) 0.4719(3) 0.031(2) Uani 1 1 d . . . C28 C 0.1746(5) 0.6977(9) 0.5550(3) 0.038(2) Uani 1 1 d . . . C29 C 0.2177(7) 0.5963(10) 0.5626(4) 0.053(3) Uani 1 1 d . . . H29A H 0.2470 0.5770 0.5374 0.064 Uiso 1 1 calc R . . H29B H 0.1844 0.5338 0.5693 0.064 Uiso 1 1 calc R . . C30 C 0.2691(7) 0.6222(13) 0.6004(4) 0.063(4) Uani 1 1 d . . . H30A H 0.3184 0.5883 0.5963 0.075 Uiso 1 1 calc R . . H30B H 0.2478 0.5934 0.6269 0.075 Uiso 1 1 calc R . . C31 C 0.2754(8) 0.7512(13) 0.6020(4) 0.067(4) Uani 1 1 d . . . H31A H 0.2712 0.7797 0.6312 0.081 Uiso 1 1 calc R . . H31B H 0.3221 0.7778 0.5894 0.081 Uiso 1 1 calc R . . C32 C 0.5735(10) 0.0346(11) 0.5466(4) 0.071(4) Uani 1 1 d . . . H32A H 0.5860 0.0359 0.5771 0.086 Uiso 1 1 calc R . . H32B H 0.5278 -0.0097 0.5428 0.086 Uiso 1 1 calc R . . C33 C 0.6308(13) -0.0140(13) 0.5245(6) 0.103(7) Uani 1 1 d . . . H33A H 0.6156 -0.0872 0.5134 0.124 Uiso 1 1 calc R . . H33B H 0.6748 -0.0238 0.5430 0.124 Uiso 1 1 calc R . . C34 C 0.6484(9) 0.0685(10) 0.4869(4) 0.062(3) Uani 1 1 d . . . H34A H 0.7019 0.0858 0.4858 0.074 Uiso 1 1 calc R . . H34B H 0.6324 0.0372 0.4594 0.074 Uiso 1 1 calc R . . C35 C 0.6036(6) 0.1699(8) 0.4979(3) 0.039(2) Uani 1 1 d . . . C36 C 0.8614(8) -0.0005(12) 0.2877(6) 0.074(4) Uani 1 1 d . . . H36A H 0.8931 -0.0146 0.3128 0.088 Uiso 1 1 calc R . . H36B H 0.8446 -0.0719 0.2757 0.088 Uiso 1 1 calc R . . C37 C 0.8995(9) 0.0649(13) 0.2568(6) 0.081(5) Uani 1 1 d . . . H37A H 0.8903 0.0351 0.2281 0.097 Uiso 1 1 calc R . . H37B H 0.9535 0.0639 0.2624 0.097 Uiso 1 1 calc R . . C38 C 0.8690(7) 0.1853(11) 0.2601(4) 0.062(3) Uani 1 1 d . . . H38A H 0.9046 0.2332 0.2755 0.074 Uiso 1 1 calc R . . H38B H 0.8601 0.2169 0.2317 0.074 Uiso 1 1 calc R . . C39 C 0.8042(6) 0.1768(9) 0.2818(3) 0.040(2) Uani 1 1 d . . . N1 N 0.2082(6) 0.7818(9) 0.5751(3) 0.056(3) Uani 1 1 d . . . H1 H 0.1924 0.8503 0.5728 0.067 Uiso 1 1 calc R . . N2 N 0.5604(6) 0.1470(8) 0.5318(3) 0.050(2) Uani 1 1 d . . . H2 H 0.5289 0.1936 0.5432 0.061 Uiso 1 1 calc R . . N3 N 0.7950(8) 0.0748(10) 0.2987(5) 0.085(4) Uani 1 1 d . . . H3A H 0.7567 0.0544 0.3138 0.102 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 0.0210(6) 0.0621(9) 0.0433(7) -0.0346(6) -0.0074(5) 0.0032(5) Zn2 0.0217(6) 0.0235(5) 0.0144(4) -0.0023(3) -0.0030(4) 0.0038(4) Zn3 0.0289(6) 0.0291(6) 0.0145(5) 0.0023(3) -0.0017(4) -0.0048(4) Zn4 0.0306(6) 0.0301(6) 0.0200(5) 0.0005(4) -0.0020(4) 0.0037(4) Zn5 0.0320(7) 0.0655(9) 0.0450(7) 0.0332(6) -0.0106(5) -0.0098(6) O1 0.071(7) 0.157(11) 0.082(7) -0.057(7) 0.030(6) -0.072(7) O2 0.069(7) 0.077(8) 0.121(10) -0.014(7) -0.002(7) -0.008(5) O3 0.181(13) 0.054(6) 0.097(8) 0.013(5) -0.101(9) -0.041(7) O4 0.053(5) 0.072(6) 0.048(4) -0.012(4) -0.021(4) -0.008(4) O5 0.073(7) 0.095(8) 0.053(5) -0.017(5) -0.014(5) -0.022(6) O6 0.058(5) 0.066(6) 0.058(5) -0.023(4) -0.027(4) -0.003(4) O7 0.133(9) 0.078(7) 0.032(4) -0.001(4) -0.016(5) 0.071(6) O8 0.047(4) 0.037(4) 0.031(3) 0.000(3) -0.008(3) 0.023(3) O9 0.064(5) 0.041(4) 0.021(3) 0.008(3) 0.012(3) 0.022(4) O10 0.069(5) 0.036(4) 0.028(3) 0.005(3) 0.001(3) 0.019(4) O11 0.039(4) 0.048(4) 0.021(3) 0.006(3) -0.005(3) 0.014(3) O12 0.038(4) 0.037(4) 0.017(3) 0.006(2) 0.006(3) 0.002(3) O13 0.036(4) 0.065(6) 0.059(5) -0.033(4) 0.001(4) 0.003(4) O14 0.037(5) 0.077(6) 0.067(5) -0.040(5) -0.003(4) 0.001(4) O15 0.030(4) 0.078(6) 0.059(5) -0.044(4) -0.003(4) 0.005(4) O16 0.033(4) 0.043(4) 0.036(3) -0.023(3) -0.005(3) 0.008(3) O17 0.023(4) 0.044(4) 0.046(4) -0.006(3) -0.004(3) -0.015(3) O18 0.034(4) 0.046(4) 0.033(3) -0.011(3) 0.001(3) 0.001(3) O19 0.044(4) 0.050(5) 0.050(4) -0.017(3) -0.019(4) -0.011(3) O20 0.043(4) 0.028(4) 0.031(3) 0.003(3) 0.004(3) 0.005(3) O21 0.049(5) 0.046(5) 0.054(4) 0.014(4) 0.011(4) 0.013(4) O22 0.041(4) 0.026(3) 0.026(3) -0.001(2) 0.000(3) 0.005(3) C1 0.057(8) 0.060(8) 0.058(7) -0.024(6) 0.017(6) -0.018(6) C2 0.059(8) 0.057(7) 0.043(6) -0.019(5) 0.009(5) -0.023(6) C3 0.051(7) 0.047(7) 0.053(6) -0.011(5) -0.014(6) -0.012(5) C4 0.065(9) 0.058(8) 0.065(8) -0.017(6) -0.025(7) -0.020(6) C5 0.030(6) 0.065(8) 0.053(6) -0.019(6) -0.007(5) -0.019(5) C6 0.036(7) 0.084(9) 0.051(7) -0.042(6) 0.005(5) -0.009(6) C7 0.041(8) 0.106(12) 0.065(9) -0.019(8) 0.026(7) -0.025(7) C8 0.055(8) 0.036(7) 0.072(8) -0.001(6) -0.017(7) -0.003(6) C9 0.043(7) 0.069(9) 0.051(7) -0.018(6) -0.010(6) -0.001(6) C10 0.074(8) 0.037(6) 0.025(4) 0.005(4) 0.000(5) 0.027(5) C11 0.051(7) 0.038(6) 0.027(4) 0.006(4) 0.010(4) 0.017(5) C12 0.051(7) 0.045(6) 0.013(4) 0.013(4) -0.001(4) 0.010(5) C13 0.041(6) 0.040(5) 0.015(4) 0.005(3) 0.008(4) 0.025(4) C14 0.028(5) 0.040(5) 0.017(4) 0.010(3) 0.008(4) 0.010(4) C15 0.038(6) 0.051(6) 0.024(4) 0.010(4) 0.003(4) 0.015(5) C16 0.030(6) 0.052(6) 0.030(5) 0.008(4) 0.008(4) 0.018(5) C17 0.037(6) 0.055(7) 0.018(4) 0.000(4) 0.012(4) 0.001(5) C18 0.023(5) 0.030(5) 0.029(4) -0.011(4) 0.011(4) 0.001(4) C19 0.030(6) 0.072(8) 0.045(6) -0.040(6) -0.002(5) 0.005(5) C20 0.041(6) 0.060(7) 0.037(5) -0.040(5) -0.006(5) 0.011(5) C21 0.019(5) 0.046(6) 0.024(4) -0.009(4) 0.000(4) -0.010(4) C22 0.020(5) 0.032(5) 0.028(4) -0.014(4) 0.000(4) 0.000(4) C23 0.035(6) 0.045(6) 0.019(4) -0.014(4) 0.005(4) 0.000(4) C24 0.023(5) 0.047(6) 0.040(5) -0.019(4) 0.002(4) -0.005(4) C25 0.042(7) 0.068(8) 0.045(6) -0.026(5) -0.001(5) 0.026(6) C26 0.018(5) 0.036(5) 0.023(4) -0.008(3) 0.002(4) -0.001(4) C27 0.030(5) 0.042(6) 0.022(4) -0.004(4) -0.001(4) 0.008(4) C28 0.027(5) 0.057(7) 0.029(5) -0.015(4) 0.001(4) -0.017(5) C29 0.040(7) 0.066(8) 0.054(7) -0.013(6) -0.014(6) 0.013(6) C30 0.050(8) 0.091(11) 0.047(7) 0.003(6) 0.002(6) 0.005(7) C31 0.059(8) 0.102(12) 0.041(6) -0.007(7) -0.001(6) 0.005(8) C32 0.114(13) 0.048(8) 0.052(7) 0.012(6) -0.001(8) -0.005(8) C33 0.18(2) 0.051(10) 0.082(11) 0.015(8) -0.022(13) 0.009(11) C34 0.084(10) 0.044(7) 0.057(7) 0.000(5) 0.016(7) 0.012(7) C35 0.053(7) 0.028(5) 0.036(5) -0.003(4) -0.003(5) 0.008(4) C36 0.060(9) 0.060(9) 0.101(12) -0.008(8) 0.011(8) 0.009(7) C37 0.073(10) 0.074(11) 0.094(11) -0.005(9) -0.020(9) 0.020(8) C38 0.056(8) 0.060(8) 0.069(8) -0.001(6) -0.013(7) 0.006(6) C39 0.047(7) 0.040(6) 0.033(5) 0.003(4) 0.006(5) 0.015(5) N1 0.056(6) 0.059(7) 0.053(5) -0.015(5) -0.023(5) -0.026(5) N2 0.074(7) 0.037(5) 0.041(5) 0.012(4) 0.018(5) 0.003(5) N3 0.096(10) 0.050(7) 0.110(11) 0.006(7) 0.033(9) -0.012(7) _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 O19 1.987(7) . ? Zn1 O6 2.011(9) . ? Zn1 O14 2.035(8) 3_566 ? Zn1 O5 2.067(11) 3_566 ? Zn1 O13 2.091(7) . ? Zn1 Zn1 2.994(3) 3_566 ? Zn2 O20 2.014(6) . ? Zn2 O17 2.016(6) . ? Zn2 O18 2.021(7) 3_666 ? Zn2 O10 2.045(7) . ? Zn2 O9 2.071(6) 3_666 ? Zn2 Zn2 3.005(2) 3_666 ? Zn3 O8 1.959(6) 2_645 ? Zn3 O22 1.984(7) . ? Zn3 O16 1.987(6) 2_655 ? Zn3 O12 1.998(6) . ? Zn4 O22 1.941(6) . ? Zn4 O21 1.941(8) . ? Zn4 O11 1.961(7) . ? Zn4 O4 1.991(8) 1_655 ? Zn5 O15 2.020(7) 2_655 ? Zn5 O3 2.053(12) 1_655 ? Zn5 O1 2.062(11) 2_645 ? Zn5 O22 2.097(7) . ? O1 C7 1.268(17) . ? O1 Zn5 2.062(11) 2_655 ? O2 C7 1.219(18) . ? O3 C8 1.264(16) . ? O3 Zn5 2.053(12) 1_455 ? O4 C8 1.287(14) . ? O4 Zn4 1.991(8) 1_455 ? O5 C9 1.240(15) . ? O5 Zn1 2.067(11) 3_566 ? O6 C9 1.254(14) . ? O7 C16 1.244(12) . ? O8 C16 1.246(12) . ? O8 Zn3 1.959(6) 2_655 ? O9 C17 1.296(11) . ? O9 Zn2 2.071(6) 3_666 ? O10 C17 1.250(12) . ? O11 C18 1.263(11) . ? O12 C18 1.271(11) . ? O13 C25 1.297(13) . ? O14 C25 1.311(15) . ? O14 Zn1 2.035(8) 3_566 ? O15 C26 1.223(11) . ? O15 Zn5 2.020(7) 2_645 ? O16 C26 1.267(11) . ? O16 Zn3 1.987(6) 2_645 ? O17 C27 1.310(12) . ? O18 C27 1.262(11) . ? O18 Zn2 2.021(7) 3_666 ? O19 C28 1.262(12) . ? O20 C35 1.270(12) . ? O21 C39 1.267(12) . ? C1 C2 1.421(16) . ? C1 C6 1.429(19) . ? C1 C7 1.461(19) . ? C2 C3 1.427(16) . ? C2 H3 0.9500 . ? C3 C4 1.392(18) . ? C3 C8 1.412(16) . ? C4 C5 1.463(15) . ? C4 H6 0.9500 . ? C5 C6 1.403(17) . ? C5 C9 1.501(18) . ? C6 H9 0.9500 . ? C10 C11 1.368(13) . ? C10 C15 1.439(14) . ? C10 C16 1.533(13) . ? C11 C12 1.434(14) . ? C11 H12 0.9500 . ? C12 C13 1.346(13) . ? C12 C17 1.518(11) . ? C13 C14 1.424(11) . ? C13 H15 0.9500 . ? C14 C15 1.390(13) . ? C14 C18 1.482(12) . ? C15 H18 0.9500 . ? C19 C24 1.366(14) . ? C19 C20 1.473(12) . ? C19 C25 1.476(15) . ? C20 C21 1.330(13) . ? C20 H21 0.9500 . ? C21 C22 1.467(12) . ? C21 C26 1.530(11) . ? C22 C23 1.426(11) . ? C22 H24 0.9500 . ? C23 C24 1.390(14) . ? C23 C27 1.467(14) . ? C24 H27 0.9500 . ? C28 N1 1.342(13) . ? C28 C29 1.472(16) . ? C29 C30 1.541(17) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.57(2) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 N1 1.523(16) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.38(2) . ? C32 N2 1.459(16) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.589(19) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.512(15) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 N2 1.361(13) . ? C36 C37 1.44(2) . ? C36 N3 1.548(19) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.561(19) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.367(16) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 N3 1.356(15) . ? N1 H1 0.8800 . ? N2 H2 0.8800 . ? N3 H3A 0.8800 . ? 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 O19 Zn1 O6 99.9(3) . . ? O19 Zn1 O14 99.4(3) . 3_566 ? O6 Zn1 O14 91.8(4) . 3_566 ? O19 Zn1 O5 102.2(4) . 3_566 ? O6 Zn1 O5 157.5(4) . 3_566 ? O14 Zn1 O5 88.9(4) 3_566 3_566 ? O19 Zn1 O13 100.4(3) . . ? O6 Zn1 O13 87.5(4) . . ? O14 Zn1 O13 160.0(3) 3_566 . ? O5 Zn1 O13 84.3(4) 3_566 . ? O19 Zn1 Zn1 169.2(2) . 3_566 ? O6 Zn1 Zn1 84.3(2) . 3_566 ? O14 Zn1 Zn1 90.4(2) 3_566 3_566 ? O5 Zn1 Zn1 73.2(3) 3_566 3_566 ? O13 Zn1 Zn1 69.6(2) . 3_566 ? O20 Zn2 O17 98.4(3) . . ? O20 Zn2 O18 103.3(3) . 3_666 ? O17 Zn2 O18 158.2(3) . 3_666 ? O20 Zn2 O10 102.8(3) . . ? O17 Zn2 O10 87.3(3) . . ? O18 Zn2 O10 88.5(3) 3_666 . ? O20 Zn2 O9 97.5(3) . 3_666 ? O17 Zn2 O9 90.1(3) . 3_666 ? O18 Zn2 O9 86.4(3) 3_666 3_666 ? O10 Zn2 O9 159.7(3) . 3_666 ? O20 Zn2 Zn2 172.55(18) . 3_666 ? O17 Zn2 Zn2 82.6(2) . 3_666 ? O18 Zn2 Zn2 75.7(2) 3_666 3_666 ? O10 Zn2 Zn2 84.6(2) . 3_666 ? O9 Zn2 Zn2 75.07(19) 3_666 3_666 ? O8 Zn3 O22 111.5(3) 2_645 . ? O8 Zn3 O16 104.8(3) 2_645 2_655 ? O22 Zn3 O16 110.2(3) . 2_655 ? O8 Zn3 O12 113.9(3) 2_645 . ? O22 Zn3 O12 108.9(3) . . ? O16 Zn3 O12 107.4(3) 2_655 . ? O22 Zn4 O21 117.8(3) . . ? O22 Zn4 O11 111.6(3) . . ? O21 Zn4 O11 109.6(3) . . ? O22 Zn4 O4 112.1(3) . 1_655 ? O21 Zn4 O4 105.0(4) . 1_655 ? O11 Zn4 O4 99.1(3) . 1_655 ? O15 Zn5 O3 112.0(4) 2_655 1_655 ? O15 Zn5 O1 96.7(4) 2_655 2_645 ? O3 Zn5 O1 149.1(5) 1_655 2_645 ? O15 Zn5 O22 95.1(3) 2_655 . ? O3 Zn5 O22 91.1(4) 1_655 . ? O1 Zn5 O22 97.9(4) 2_645 . ? C7 O1 Zn5 101.0(10) . 2_655 ? C8 O3 Zn5 127.2(10) . 1_455 ? C8 O4 Zn4 121.9(8) . 1_455 ? C9 O5 Zn1 135.8(8) . 3_566 ? C9 O6 Zn1 123.2(9) . . ? C16 O8 Zn3 109.0(6) . 2_655 ? C17 O9 Zn2 131.3(6) . 3_666 ? C17 O10 Zn2 121.0(6) . . ? C18 O11 Zn4 131.0(6) . . ? C18 O12 Zn3 126.5(6) . . ? C25 O13 Zn1 141.4(8) . . ? C25 O14 Zn1 116.4(7) . 3_566 ? C26 O15 Zn5 144.3(6) . 2_645 ? C26 O16 Zn3 125.7(6) . 2_645 ? C27 O17 Zn2 124.7(6) . . ? C27 O18 Zn2 134.7(6) . 3_666 ? C28 O19 Zn1 128.5(7) . . ? C35 O20 Zn2 131.3(6) . . ? C39 O21 Zn4 134.3(7) . . ? Zn4 O22 Zn3 107.3(3) . . ? Zn4 O22 Zn5 110.9(3) . . ? Zn3 O22 Zn5 114.3(3) . . ? C2 C1 C6 121.0(11) . . ? C2 C1 C7 120.6(12) . . ? C6 C1 C7 118.2(12) . . ? C1 C2 C3 120.6(11) . . ? C1 C2 H3 119.7 . . ? C3 C2 H3 119.7 . . ? C4 C3 C8 118.3(11) . . ? C4 C3 C2 119.4(10) . . ? C8 C3 C2 122.2(11) . . ? C3 C4 C5 119.4(12) . . ? C3 C4 H6 120.3 . . ? C5 C4 H6 120.3 . . ? C6 C5 C4 121.9(11) . . ? C6 C5 C9 119.7(10) . . ? C4 C5 C9 118.4(11) . . ? C5 C6 C1 117.5(10) . . ? C5 C6 H9 121.2 . . ? C1 C6 H9 121.2 . . ? O2 C7 O1 121.9(14) . . ? O2 C7 C1 119.6(13) . . ? O1 C7 C1 118.3(14) . . ? O3 C8 O4 120.1(11) . . ? O3 C8 C3 122.2(12) . . ? O4 C8 C3 117.6(11) . . ? O5 C9 O6 123.5(12) . . ? O5 C9 C5 117.4(10) . . ? O6 C9 C5 118.6(12) . . ? C11 C10 C15 120.1(9) . . ? C11 C10 C16 121.0(9) . . ? C15 C10 C16 118.9(8) . . ? C10 C11 C12 120.3(9) . . ? C10 C11 H12 119.9 . . ? C12 C11 H12 119.9 . . ? C13 C12 C11 119.2(8) . . ? C13 C12 C17 120.6(9) . . ? C11 C12 C17 120.2(8) . . ? C12 C13 C14 122.3(8) . . ? C12 C13 H15 118.9 . . ? C14 C13 H15 118.9 . . ? C15 C14 C13 118.8(8) . . ? C15 C14 C18 121.6(8) . . ? C13 C14 C18 119.6(8) . . ? C14 C15 C10 119.3(8) . . ? C14 C15 H18 120.4 . . ? C10 C15 H18 120.4 . . ? O7 C16 O8 125.2(9) . . ? O7 C16 C10 117.8(9) . . ? O8 C16 C10 117.0(8) . . ? O10 C17 O9 127.2(8) . . ? O10 C17 C12 116.5(8) . . ? O9 C17 C12 116.2(9) . . ? O11 C18 O12 125.5(8) . . ? O11 C18 C14 116.7(8) . . ? O12 C18 C14 117.6(8) . . ? C24 C19 C20 119.5(9) . . ? C24 C19 C25 120.2(9) . . ? C20 C19 C25 120.4(10) . . ? C21 C20 C19 117.5(9) . . ? C21 C20 H21 121.2 . . ? C19 C20 H21 121.2 . . ? C20 C21 C22 124.2(8) . . ? C20 C21 C26 118.5(8) . . ? C22 C21 C26 116.6(7) . . ? C23 C22 C21 114.8(8) . . ? C23 C22 H24 122.6 . . ? C21 C22 H24 122.6 . . ? C24 C23 C22 121.1(9) . . ? C24 C23 C27 119.5(8) . . ? C22 C23 C27 119.3(8) . . ? C19 C24 C23 121.9(9) . . ? C19 C24 H27 119.0 . . ? C23 C24 H27 119.0 . . ? O13 C25 O14 122.1(9) . . ? O13 C25 C19 115.3(11) . . ? O14 C25 C19 122.6(10) . . ? O15 C26 O16 125.1(8) . . ? O15 C26 C21 115.6(8) . . ? O16 C26 C21 119.2(8) . . ? O18 C27 O17 122.0(9) . . ? O18 C27 C23 119.1(8) . . ? O17 C27 C23 118.8(8) . . ? O19 C28 N1 123.0(11) . . ? O19 C28 C29 128.2(9) . . ? N1 C28 C29 108.6(10) . . ? C28 C29 C30 105.8(10) . . ? C28 C29 H29A 110.6 . . ? C30 C29 H29A 110.6 . . ? C28 C29 H29B 110.6 . . ? C30 C29 H29B 110.6 . . ? H29A C29 H29B 108.7 . . ? C29 C30 C31 105.7(11) . . ? C29 C30 H30A 110.6 . . ? C31 C30 H30A 110.6 . . ? C29 C30 H30B 110.6 . . ? C31 C30 H30B 110.6 . . ? H30A C30 H30B 108.7 . . ? N1 C31 C30 99.6(11) . . ? N1 C31 H31A 111.9 . . ? C30 C31 H31A 111.9 . . ? N1 C31 H31B 111.9 . . ? C30 C31 H31B 111.9 . . ? H31A C31 H31B 109.6 . . ? C33 C32 N2 110.8(12) . . ? C33 C32 H32A 109.5 . . ? N2 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? N2 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? C32 C33 C34 105.4(13) . . ? C32 C33 H33A 110.7 . . ? C34 C33 H33A 110.7 . . ? C32 C33 H33B 110.7 . . ? C34 C33 H33B 110.7 . . ? H33A C33 H33B 108.8 . . ? C35 C34 C33 103.1(11) . . ? C35 C34 H34A 111.1 . . ? C33 C34 H34A 111.1 . . ? C35 C34 H34B 111.1 . . ? C33 C34 H34B 111.1 . . ? H34A C34 H34B 109.1 . . ? O20 C35 N2 124.2(9) . . ? O20 C35 C34 126.6(9) . . ? N2 C35 C34 109.2(9) . . ? C37 C36 N3 101.8(12) . . ? C37 C36 H36A 111.4 . . ? N3 C36 H36A 111.4 . . ? C37 C36 H36B 111.4 . . ? N3 C36 H36B 111.4 . . ? H36A C36 H36B 109.3 . . ? C36 C37 C38 107.2(13) . . ? C36 C37 H37A 110.3 . . ? C38 C37 H37A 110.3 . . ? C36 C37 H37B 110.3 . . ? C38 C37 H37B 110.3 . . ? H37A C37 H37B 108.5 . . ? C39 C38 C37 105.5(12) . . ? C39 C38 H38A 110.6 . . ? C37 C38 H38A 110.6 . . ? C39 C38 H38B 110.6 . . ? C37 C38 H38B 110.6 . . ? H38A C38 H38B 108.8 . . ? O21 C39 N3 123.3(11) . . ? O21 C39 C38 124.6(11) . . ? N3 C39 C38 112.0(11) . . ? C28 N1 C31 115.9(11) . . ? C28 N1 H1 122.1 . . ? C31 N1 H1 122.1 . . ? C35 N2 C32 110.5(10) . . ? C35 N2 H2 124.7 . . ? C32 N2 H2 124.7 . . ? C39 N3 C36 110.5(11) . . ? C39 N3 H3A 124.8 . . ? C36 N3 H3A 124.8 . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.761 0.107 0.160 3193.2 1972.0 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.988 _refine_diff_density_min -2.283 _refine_diff_density_rms 0.319 #end data_3 _database_code_depnum_ccdc_archive 'CCDC 868810' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 N2 O14 Zn3,C5 H9 O N' _chemical_formula_sum 'C33 H33 N3 O15 Zn3' _chemical_formula_weight 907.806 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.906(4) _cell_length_b 12.606(4) _cell_length_c 27.737(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.970(7) _cell_angle_gamma 90.00 _cell_volume 4507(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas colorless _exptl_crystal_density_diffrn 0.970 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 1.622 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.6418 _exptl_absorpt_correction_T_max 0.7373 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; O13 O14 and O15 represent the O atoms of the coordinated mpyrol molecules, the electron density remains is attributed to the disordered groups of the coordinated mpyrol solvents. ; _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 34228 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10172 _reflns_number_gt 7516 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SMART and SAINT (Siemens,1994)' _computing_data_reduction 'SMART and SAINT (Siemens,1994)' _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1697P)^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 10172 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.2351 _refine_ls_wR_factor_gt 0.2221 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 0.10239(4) 1.04485(4) 0.134328(18) 0.02869(17) Uani 1 1 d . . . Zn2 Zn -0.04182(4) 1.20078(4) 0.209824(19) 0.03170(18) Uani 1 1 d . . . Zn3 Zn -0.42813(4) 1.57719(4) 0.026072(18) 0.02668(17) Uani 1 1 d . . . O1 O 0.3928(3) 0.7597(3) 0.29939(15) 0.0527(10) Uani 1 1 d . . . O2 O 0.3224(3) 0.6784(3) 0.36151(14) 0.0502(10) Uani 1 1 d . . . O3 O -0.0112(3) 1.0210(3) 0.41360(12) 0.0442(9) Uani 1 1 d . . . O4 O 0.0930(3) 0.9060(3) 0.45378(12) 0.0433(9) Uani 1 1 d . . . O5 O 0.1284(3) 0.9828(3) 0.20053(12) 0.0446(9) Uani 1 1 d . . . O6 O 0.0267(3) 1.0809(3) 0.24489(14) 0.0504(10) Uani 1 1 d . . . O7 O -0.1167(4) 0.9558(4) -0.04600(19) 0.0751(16) Uani 1 1 d . . . O8 O -0.1679(4) 1.0743(3) -0.09857(14) 0.0557(11) Uani 1 1 d . . . O9 O -0.1016(3) 1.2335(3) 0.14455(13) 0.0447(9) Uani 1 1 d . . . O10 O -0.0464(3) 1.0750(3) 0.12238(15) 0.0432(9) Uani 1 1 d . . . O11 O -0.4408(3) 1.3285(3) -0.01726(14) 0.0482(10) Uani 1 1 d . . . O12 O -0.3398(3) 1.4407(3) 0.02592(15) 0.0449(9) Uani 1 1 d . . . O13 O -0.0642(4) 1.3258(5) 0.2507(2) 0.098(2) Uani 1 1 d . . . O14 O -0.3231(3) 1.6793(3) 0.05275(14) 0.0416(8) Uani 1 1 d . . . O15 O -0.1803(4) 1.1305(5) 0.2294(2) 0.0791(15) Uani 1 1 d . . . C1 C 0.2369(4) 0.8260(4) 0.32764(16) 0.0292(9) Uani 1 1 d . . . C2 C 0.1853(4) 0.8465(4) 0.36974(16) 0.0321(10) Uani 1 1 d . . . H2A H 0.2035 0.8080 0.3984 0.039 Uiso 1 1 calc R . . C3 C 0.1077(4) 0.9227(4) 0.36993(16) 0.0295(9) Uani 1 1 d . . . C4 C 0.0785(4) 0.9756(4) 0.32712(16) 0.0335(10) Uani 1 1 d . . . H4A H 0.0257 1.0281 0.3270 0.040 Uiso 1 1 calc R . . C5 C 0.1263(4) 0.9521(4) 0.28474(17) 0.0317(10) Uani 1 1 d . . . C6 C 0.2078(4) 0.8798(4) 0.28568(16) 0.0318(10) Uani 1 1 d . . . H6A H 0.2439 0.8674 0.2572 0.038 Uiso 1 1 calc R . . C7 C 0.3247(4) 0.7496(4) 0.32905(17) 0.0362(11) Uani 1 1 d . . . C8 C 0.0593(4) 0.9510(4) 0.41588(17) 0.0301(9) Uani 1 1 d . . . C9 C 0.0907(4) 1.0094(4) 0.23951(16) 0.0319(10) Uani 1 1 d . . . C10 C -0.1847(4) 1.1181(4) -0.01640(17) 0.0347(10) Uani 1 1 d . . . C11 C -0.1349(4) 1.1052(4) 0.02835(18) 0.0337(10) Uani 1 1 d . . . H11A H -0.0876 1.0481 0.0336 0.040 Uiso 1 1 calc R . . C12 C -0.1530(4) 1.1750(4) 0.06599(17) 0.0313(9) Uani 1 1 d . . . C13 C -0.2231(4) 1.2583(4) 0.05823(16) 0.0310(9) Uani 1 1 d . . . H13A H -0.2332 1.3083 0.0832 0.037 Uiso 1 1 calc R . . C14 C -0.2790(4) 1.2682(4) 0.01361(17) 0.0340(10) Uani 1 1 d . . . C15 C -0.2587(4) 1.1962(4) -0.02341(16) 0.0326(10) Uani 1 1 d . . . H15A H -0.2965 1.2014 -0.0536 0.039 Uiso 1 1 calc R . . C16 C -0.1571(4) 1.0447(4) -0.0564(2) 0.0409(12) Uani 1 1 d . . . C17 C -0.0957(4) 1.1611(4) 0.11437(17) 0.0327(10) Uani 1 1 d . . . C18 C -0.3600(4) 1.3545(4) 0.00698(17) 0.0344(10) 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 0.0333(3) 0.0290(3) 0.0238(3) -0.0022(2) 0.0011(2) 0.00161(19) Zn2 0.0343(3) 0.0351(3) 0.0254(3) 0.0008(2) -0.0008(2) 0.0039(2) Zn3 0.0297(3) 0.0273(3) 0.0231(3) -0.00075(19) 0.0019(2) -0.00081(19) O1 0.047(2) 0.057(2) 0.056(2) 0.016(2) 0.0182(19) 0.0180(18) O2 0.056(2) 0.053(2) 0.043(2) 0.0137(18) 0.0128(18) 0.0249(19) O3 0.052(2) 0.052(2) 0.0288(18) -0.0058(16) 0.0088(16) 0.0119(18) O4 0.056(2) 0.049(2) 0.0255(17) 0.0024(15) 0.0073(16) 0.0086(17) O5 0.049(2) 0.060(2) 0.0247(17) 0.0058(16) 0.0028(15) 0.0141(18) O6 0.053(2) 0.060(3) 0.038(2) 0.0182(18) 0.0067(17) 0.0255(19) O7 0.089(4) 0.066(3) 0.069(3) -0.023(3) -0.014(3) 0.039(3) O8 0.079(3) 0.055(3) 0.034(2) -0.0148(18) 0.006(2) 0.010(2) O9 0.058(2) 0.043(2) 0.0314(18) -0.0029(16) -0.0076(16) 0.0028(17) O10 0.0325(19) 0.041(2) 0.055(2) 0.0108(17) -0.0117(16) 0.0031(14) O11 0.042(2) 0.055(2) 0.047(2) -0.0058(18) -0.0044(17) 0.0210(18) O12 0.047(2) 0.0348(19) 0.052(2) -0.0005(17) -0.0051(18) 0.0095(15) O13 0.062(3) 0.115(5) 0.117(5) -0.071(4) 0.011(3) -0.009(3) O14 0.0401(19) 0.041(2) 0.044(2) -0.0087(16) 0.0040(16) -0.0103(15) O15 0.051(3) 0.099(4) 0.087(4) 0.021(3) 0.000(3) -0.008(3) C1 0.034(2) 0.031(2) 0.022(2) 0.0007(17) 0.0060(17) 0.0037(18) C2 0.042(3) 0.030(2) 0.024(2) 0.0020(18) -0.0005(19) 0.0084(19) C3 0.031(2) 0.036(2) 0.021(2) 0.0011(17) 0.0026(17) 0.0008(18) C4 0.034(2) 0.037(2) 0.030(2) 0.002(2) 0.0033(19) 0.0095(19) C5 0.035(2) 0.034(2) 0.026(2) 0.0039(18) 0.0011(18) 0.0026(18) C6 0.034(2) 0.039(3) 0.023(2) 0.0005(19) 0.0073(18) 0.0019(19) C7 0.040(3) 0.035(3) 0.033(2) 0.001(2) 0.002(2) 0.007(2) C8 0.030(2) 0.033(2) 0.027(2) 0.0000(18) 0.0028(18) -0.0015(17) C9 0.035(2) 0.038(2) 0.022(2) 0.0061(18) -0.0010(18) -0.0011(19) C10 0.038(3) 0.036(2) 0.031(2) -0.012(2) 0.0033(19) -0.0019(19) C11 0.033(2) 0.030(2) 0.038(3) -0.005(2) -0.0015(19) 0.0077(18) C12 0.031(2) 0.037(2) 0.025(2) -0.0018(18) -0.0034(17) 0.0046(18) C13 0.034(2) 0.028(2) 0.031(2) -0.0057(18) -0.0052(19) 0.0071(18) C14 0.039(3) 0.036(2) 0.027(2) 0.0015(19) 0.0013(19) 0.007(2) C15 0.035(2) 0.041(3) 0.022(2) -0.0009(18) 0.0001(18) 0.0053(19) C16 0.031(2) 0.050(3) 0.041(3) -0.018(2) -0.004(2) -0.003(2) C17 0.035(2) 0.037(3) 0.025(2) 0.0031(19) -0.0036(18) -0.0026(19) C18 0.036(2) 0.041(3) 0.026(2) 0.000(2) -0.0006(19) 0.011(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 O2 1.944(4) 2 ? Zn1 O10 1.969(4) . ? Zn1 O5 2.008(4) . ? Zn1 O8 2.010(4) 3_575 ? Zn1 O7 2.467(5) 3_575 ? Zn1 C16 2.570(5) 3_575 ? Zn2 O13 1.971(5) . ? Zn2 O9 1.975(4) . ? Zn2 O6 1.980(4) . ? Zn2 O1 2.090(4) 2 ? Zn2 O15 2.092(5) . ? Zn3 O14 1.985(4) . ? Zn3 O3 2.013(3) 2_455 ? Zn3 O4 2.049(3) 4_585 ? Zn3 O12 2.064(4) . ? Zn3 O11 2.072(4) 3_485 ? Zn3 Zn3 3.0071(12) 3_485 ? O1 C7 1.241(6) . ? O1 Zn2 2.090(4) 2_545 ? O2 C7 1.272(6) . ? O2 Zn1 1.944(4) 2_545 ? O3 C8 1.267(6) . ? O3 Zn3 2.013(3) 2_445 ? O4 C8 1.252(6) . ? O4 Zn3 2.049(3) 4_686 ? O5 C9 1.254(6) . ? O6 C9 1.238(6) . ? O7 C16 1.263(7) . ? O7 Zn1 2.467(5) 3_575 ? O8 C16 1.229(7) . ? O8 Zn1 2.010(4) 3_575 ? O9 C17 1.243(6) . ? O10 C17 1.272(6) . ? O11 C18 1.254(7) . ? O11 Zn3 2.072(4) 3_485 ? O12 C18 1.229(6) . ? C1 C6 1.382(6) . ? C1 C2 1.398(6) . ? C1 C7 1.486(6) . ? C2 C3 1.389(6) . ? C2 H2A 0.9500 . ? C3 C4 1.396(6) . ? C3 C8 1.491(6) . ? C4 C5 1.387(6) . ? C4 H4A 0.9500 . ? C5 C6 1.391(7) . ? C5 C9 1.499(6) . ? C6 H6A 0.9500 . ? C10 C11 1.377(7) . ? C10 C15 1.379(7) . ? C10 C16 1.501(6) . ? C11 C12 1.394(6) . ? C11 H11A 0.9500 . ? C12 C13 1.396(6) . ? C12 C17 1.508(6) . ? C13 C14 1.405(7) . ? C13 H13A 0.9500 . ? C14 C15 1.405(6) . ? C14 C18 1.513(7) . ? C15 H15A 0.9500 . ? C16 Zn1 2.570(5) 3_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O10 108.83(17) 2 . ? O2 Zn1 O5 102.93(18) 2 . ? O10 Zn1 O5 110.16(16) . . ? O2 Zn1 O8 117.03(19) 2 3_575 ? O10 Zn1 O8 119.52(19) . 3_575 ? O5 Zn1 O8 96.05(17) . 3_575 ? O2 Zn1 O7 89.93(18) 2 3_575 ? O10 Zn1 O7 87.49(17) . 3_575 ? O5 Zn1 O7 152.78(15) . 3_575 ? O8 Zn1 O7 56.78(16) 3_575 3_575 ? O2 Zn1 C16 105.80(17) 2 3_575 ? O10 Zn1 C16 104.54(17) . 3_575 ? O5 Zn1 C16 123.90(18) . 3_575 ? O8 Zn1 C16 27.85(18) 3_575 3_575 ? O7 Zn1 C16 28.95(17) 3_575 3_575 ? O13 Zn2 O9 107.4(3) . . ? O13 Zn2 O6 113.7(3) . . ? O9 Zn2 O6 138.86(17) . . ? O13 Zn2 O1 87.1(2) . 2 ? O9 Zn2 O1 97.60(18) . 2 ? O6 Zn2 O1 86.61(19) . 2 ? O13 Zn2 O15 92.1(3) . . ? O9 Zn2 O15 91.60(19) . . ? O6 Zn2 O15 85.1(2) . . ? O1 Zn2 O15 170.6(2) 2 . ? O14 Zn3 O3 101.89(16) . 2_455 ? O14 Zn3 O4 100.06(16) . 4_585 ? O3 Zn3 O4 158.05(16) 2_455 4_585 ? O14 Zn3 O12 100.06(16) . . ? O3 Zn3 O12 86.95(17) 2_455 . ? O4 Zn3 O12 89.00(16) 4_585 . ? O14 Zn3 O11 102.12(17) . 3_485 ? O3 Zn3 O11 87.11(17) 2_455 3_485 ? O4 Zn3 O11 88.56(16) 4_585 3_485 ? O12 Zn3 O11 157.77(17) . 3_485 ? O14 Zn3 Zn3 172.56(11) . 3_485 ? O3 Zn3 Zn3 85.13(11) 2_455 3_485 ? O4 Zn3 Zn3 72.93(11) 4_585 3_485 ? O12 Zn3 Zn3 77.67(12) . 3_485 ? O11 Zn3 Zn3 80.49(12) 3_485 3_485 ? C7 O1 Zn2 137.1(4) . 2_545 ? C7 O2 Zn1 128.5(3) . 2_545 ? C8 O3 Zn3 120.9(3) . 2_445 ? C8 O4 Zn3 135.8(3) . 4_686 ? C9 O5 Zn1 129.1(3) . . ? C9 O6 Zn2 141.3(3) . . ? C16 O7 Zn1 80.1(4) . 3_575 ? C16 O8 Zn1 102.3(4) . 3_575 ? C17 O9 Zn2 115.4(3) . . ? C17 O10 Zn1 131.9(3) . . ? C18 O11 Zn3 124.4(3) . 3_485 ? C18 O12 Zn3 129.3(3) . . ? C6 C1 C2 119.5(4) . . ? C6 C1 C7 120.9(4) . . ? C2 C1 C7 119.6(4) . . ? C3 C2 C1 120.4(4) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? C2 C3 C4 119.3(4) . . ? C2 C3 C8 120.2(4) . . ? C4 C3 C8 120.5(4) . . ? C5 C4 C3 120.5(4) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? C4 C5 C6 119.5(4) . . ? C4 C5 C9 118.4(4) . . ? C6 C5 C9 122.0(4) . . ? C1 C6 C5 120.6(4) . . ? C1 C6 H6A 119.7 . . ? C5 C6 H6A 119.7 . . ? O1 C7 O2 125.8(5) . . ? O1 C7 C1 118.8(4) . . ? O2 C7 C1 115.4(4) . . ? O4 C8 O3 125.1(4) . . ? O4 C8 C3 117.9(4) . . ? O3 C8 C3 117.1(4) . . ? O6 C9 O5 126.2(4) . . ? O6 C9 C5 115.3(4) . . ? O5 C9 C5 118.5(4) . . ? C11 C10 C15 119.9(4) . . ? C11 C10 C16 118.4(5) . . ? C15 C10 C16 121.7(5) . . ? C10 C11 C12 120.8(4) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C11 C12 C13 119.4(4) . . ? C11 C12 C17 120.0(4) . . ? C13 C12 C17 120.5(4) . . ? C12 C13 C14 120.1(4) . . ? C12 C13 H13A 119.9 . . ? C14 C13 H13A 119.9 . . ? C15 C14 C13 118.7(4) . . ? C15 C14 C18 121.9(4) . . ? C13 C14 C18 119.4(4) . . ? C10 C15 C14 120.8(4) . . ? C10 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? O8 C16 O7 120.8(5) . . ? O8 C16 C10 119.8(5) . . ? O7 C16 C10 119.2(5) . . ? O8 C16 Zn1 49.8(3) . 3_575 ? O7 C16 Zn1 71.0(3) . 3_575 ? C10 C16 Zn1 168.0(4) . 3_575 ? O9 C17 O10 123.8(5) . . ? O9 C17 C12 118.0(4) . . ? O10 C17 C12 118.1(4) . . ? O12 C18 O11 127.7(5) . . ? O12 C18 C14 116.9(5) . . ? O11 C18 C14 115.3(5) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.432 0.017 -0.005 2814.9 484.8 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 5.529 _refine_diff_density_min -0.941 _refine_diff_density_rms 0.169 #end data_4 _database_code_depnum_ccdc_archive 'CCDC 886076' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H36 N6 O15 Zn3' _chemical_formula_sum 'C33 H36 N6 O15 Zn3' _chemical_formula_weight 952.85 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 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 31.171(12) _cell_length_b 12.186(4) _cell_length_c 27.629(11) _cell_angle_alpha 90.00 _cell_angle_beta 108.264(4) _cell_angle_gamma 90.00 _cell_volume 9966(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16541 _cell_measurement_theta_min 2.0502 _cell_measurement_theta_max 27.4006 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3295 _exptl_absorpt_coefficient_mu 1.483 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.7558 _exptl_absorpt_correction_T_max 0.8082 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; O14 represent the O atom of the coordinated dmi molecule, the electron density remains is attributed to the disordered groups of the coordinated dmi solvent. Because of the free guest molecules are unknown in the compound, so the correct and complete framework formular should be [Zn3(btc)2(dmi)3](solvent)x ; _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 41899 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0943 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.39 _reflns_number_total 11234 _reflns_number_gt 7965 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SMART and SAINT (Siemens,1994)' _computing_data_reduction 'SMART and SAINT (Siemens,1994)' _computing_structure_solution SHELXTL _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 11234 _refine_ls_number_parameters 451 _refine_ls_number_restraints 136 _refine_ls_R_factor_all 0.1055 _refine_ls_R_factor_gt 0.0856 _refine_ls_wR_factor_ref 0.2858 _refine_ls_wR_factor_gt 0.2601 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 1.863 _refine_ls_shift/su_max 0.008 _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 -0.26053(4) -0.10204(9) -0.12114(4) 0.0255(4) Uani 1 1 d . . . Zn2 Zn -0.17960(4) 0.08829(10) -0.12459(4) 0.0280(4) Uani 1 1 d . . . Zn3 Zn -0.52529(4) 0.24041(11) -0.32038(5) 0.0342(4) Uani 1 1 d . . . O1 O -0.2183(3) -0.0681(8) -0.0526(3) 0.047(2) Uani 1 1 d . . . O2 O -0.1657(3) 0.0582(7) -0.0509(3) 0.042(2) Uani 1 1 d . . . O3 O -0.0659(3) 0.1813(8) 0.1192(3) 0.050(2) Uani 1 1 d . . . O4 O -0.0559(4) 0.0749(10) 0.1868(4) 0.067(3) Uani 1 1 d . . . O5 O -0.1597(5) -0.2469(11) 0.1720(4) 0.084(4) Uani 1 1 d . . . O6 O -0.2047(3) -0.2965(7) 0.0954(3) 0.044(2) Uani 1 1 d . . . O7 O -0.2918(3) 0.0300(7) -0.1567(3) 0.0387(18) Uani 1 1 d . . . O8 O -0.2361(3) 0.0897(7) -0.1851(3) 0.0362(18) Uani 1 1 d . . . O9 O -0.2698(3) 0.3307(7) -0.3339(3) 0.0426(19) Uani 1 1 d . . . O10 O -0.3347(3) 0.4294(7) -0.3571(3) 0.0406(19) Uani 1 1 d . . . O11 O -0.4613(3) 0.2838(7) -0.2995(3) 0.044(2) Uani 1 1 d . . . O12 O -0.4428(3) 0.1886(7) -0.2260(3) 0.046(2) Uani 1 1 d . . . O13 O -0.1969(4) 0.2478(7) -0.1120(4) 0.058(3) Uani 1 1 d . . . O14 O -0.1233(3) 0.1397(9) -0.1359(4) 0.059(3) Uani 1 1 d . . . O15 O -0.5148(5) 0.0962(9) -0.3472(6) 0.081(4) Uani 1 1 d . . . C1 C -0.1621(3) -0.0334(8) 0.0260(4) 0.028(2) Uani 1 1 d . . . C2 C -0.1284(4) 0.0346(9) 0.0547(4) 0.033(2) Uani 1 1 d . . . H2A H -0.1185 0.0928 0.0391 0.039 Uiso 1 1 calc R . . C3 C -0.1087(4) 0.0169(9) 0.1075(4) 0.033(2) Uani 1 1 d . . . C4 C -0.1225(4) -0.0749(9) 0.1297(4) 0.032(2) Uani 1 1 d . . . H4A H -0.1086 -0.0899 0.1640 0.039 Uiso 1 1 calc R . . C5 C -0.1569(4) -0.1438(9) 0.1008(4) 0.031(2) Uani 1 1 d . . . C6 C -0.1767(4) -0.1221(9) 0.0482(4) 0.033(2) Uani 1 1 d . . . H6A H -0.1994 -0.1675 0.0284 0.040 Uiso 1 1 calc R . . C7 C -0.1835(4) -0.0135(9) -0.0305(4) 0.031(2) Uani 1 1 d . . . C8 C -0.0749(4) 0.0942(10) 0.1390(4) 0.038(3) Uani 1 1 d . . . C9 C -0.1746(5) -0.2373(10) 0.1260(4) 0.042(3) Uani 1 1 d . . . C10 C -0.3095(3) 0.1561(8) -0.2254(4) 0.028(2) Uani 1 1 d . . . C11 C -0.2947(4) 0.2175(9) -0.2609(4) 0.031(2) Uani 1 1 d . . . H11A H -0.2649 0.2127 -0.2608 0.037 Uiso 1 1 calc R . . C12 C -0.3251(3) 0.2848(9) -0.2957(4) 0.030(2) Uani 1 1 d . . . C13 C -0.3700(3) 0.2920(9) -0.2967(4) 0.031(2) Uani 1 1 d . . . H13A H -0.3900 0.3377 -0.3200 0.038 Uiso 1 1 calc R . . C14 C -0.3846(3) 0.2298(9) -0.2622(4) 0.031(2) Uani 1 1 d . . . C15 C -0.3545(3) 0.1644(9) -0.2262(4) 0.030(2) Uani 1 1 d . . . H15A H -0.3642 0.1258 -0.2025 0.036 Uiso 1 1 calc R . . C16 C -0.2766(4) 0.0870(8) -0.1863(4) 0.029(2) Uani 1 1 d . . . C17 C -0.3088(3) 0.3528(9) -0.3317(4) 0.030(2) Uani 1 1 d . . . C18 C -0.4330(4) 0.2365(9) -0.2618(4) 0.032(2) Uani 1 1 d . . . C19 C -0.2245(7) 0.3177(15) -0.1345(8) 0.074(2) Uani 1 1 d U . . C20 C -0.2831(7) 0.2904(16) -0.0928(8) 0.080(3) Uani 1 1 d U . . C21 C -0.2893(8) 0.4280(15) -0.1637(8) 0.080(3) Uani 1 1 d U . . C22 C -0.2561(7) 0.4638(15) -0.1899(8) 0.080(3) Uani 1 1 d U . . C23 C -0.1819(7) 0.3864(15) -0.1923(8) 0.079(3) Uani 1 1 d U . . C24 C -0.5157(10) -0.005(2) -0.3391(13) 0.128(5) Uani 1 1 d U . . C25 C -0.6009(11) -0.020(3) -0.3713(13) 0.137(10) Uani 1 1 d U . . C26 C -0.5464(10) -0.172(2) -0.3373(13) 0.133(5) Uani 1 1 d U . . C27 C -0.4928(10) -0.182(2) -0.3274(13) 0.134(5) Uani 1 1 d U . . C28 C -0.4353(12) -0.025(3) -0.316(2) 0.197(5) Uani 1 1 d U . . N1 N -0.2635(6) 0.3489(13) -0.1260(6) 0.079(2) Uani 1 1 d U . . N2 N -0.2202(6) 0.3834(12) -0.1746(7) 0.078(2) Uani 1 1 d U . . N3 N -0.5541(9) -0.0626(17) -0.3434(10) 0.129(5) Uani 1 1 d U . . N4 N -0.4821(9) -0.0712(18) -0.3223(11) 0.132(5) Uani 1 1 d U . . 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 0.0241(7) 0.0328(7) 0.0201(6) 0.0027(4) 0.0075(5) 0.0005(4) Zn2 0.0240(7) 0.0365(7) 0.0231(6) 0.0031(4) 0.0070(5) 0.0007(4) Zn3 0.0214(7) 0.0463(8) 0.0333(7) 0.0020(5) 0.0063(5) 0.0082(5) O1 0.041(5) 0.071(6) 0.023(4) -0.001(4) 0.003(3) -0.018(4) O2 0.058(6) 0.041(4) 0.024(4) 0.004(3) 0.008(3) -0.016(4) O3 0.043(5) 0.064(6) 0.036(4) -0.002(4) 0.004(4) -0.024(4) O4 0.059(7) 0.087(8) 0.036(5) 0.008(5) -0.012(5) -0.025(6) O5 0.102(10) 0.106(10) 0.034(5) 0.025(5) 0.006(6) -0.046(8) O6 0.050(5) 0.045(5) 0.038(4) 0.004(4) 0.018(4) -0.014(4) O7 0.032(4) 0.050(5) 0.038(4) 0.019(4) 0.016(3) 0.010(3) O8 0.021(4) 0.052(5) 0.032(4) 0.008(3) 0.004(3) 0.007(3) O9 0.035(4) 0.061(5) 0.037(4) 0.011(4) 0.018(3) 0.001(4) O10 0.033(4) 0.043(4) 0.041(4) 0.011(4) 0.005(4) -0.006(3) O11 0.019(4) 0.057(5) 0.054(5) 0.018(4) 0.008(3) 0.004(3) O12 0.030(4) 0.058(5) 0.056(5) 0.025(4) 0.024(4) 0.009(4) O13 0.076(8) 0.037(5) 0.055(6) 0.002(4) 0.011(5) 0.012(4) O14 0.036(5) 0.069(6) 0.081(7) 0.011(5) 0.032(5) -0.001(4) O15 0.104(11) 0.055(7) 0.113(11) -0.016(6) 0.075(9) 0.000(6) C1 0.028(5) 0.032(5) 0.021(4) 0.000(4) 0.003(4) -0.003(4) C2 0.030(5) 0.042(6) 0.026(5) 0.001(4) 0.009(4) -0.003(4) C3 0.029(5) 0.044(6) 0.023(5) -0.005(4) 0.006(4) -0.006(4) C4 0.032(6) 0.040(6) 0.024(5) 0.002(4) 0.007(4) -0.003(4) C5 0.032(5) 0.036(6) 0.026(5) 0.002(4) 0.009(4) -0.003(4) C6 0.031(5) 0.041(6) 0.026(5) -0.001(4) 0.007(4) -0.003(4) C7 0.039(6) 0.033(5) 0.021(4) -0.001(4) 0.010(4) -0.001(4) C8 0.022(5) 0.055(7) 0.033(6) -0.009(5) 0.005(4) -0.009(4) C9 0.049(7) 0.048(7) 0.032(6) 0.003(5) 0.017(5) -0.015(5) C10 0.020(5) 0.035(5) 0.028(5) 0.011(4) 0.006(4) 0.004(4) C11 0.022(5) 0.037(5) 0.033(5) 0.004(4) 0.009(4) 0.000(4) C12 0.021(5) 0.039(6) 0.031(5) 0.007(4) 0.009(4) -0.002(4) C13 0.020(5) 0.037(6) 0.036(5) 0.008(4) 0.006(4) 0.001(4) C14 0.021(5) 0.044(6) 0.029(5) 0.013(4) 0.007(4) 0.002(4) C15 0.020(5) 0.041(6) 0.028(5) 0.013(4) 0.007(4) 0.003(4) C16 0.029(5) 0.029(5) 0.027(5) 0.002(4) 0.007(4) 0.001(4) C17 0.024(5) 0.042(6) 0.022(4) 0.004(4) 0.005(4) -0.005(4) C18 0.023(5) 0.040(6) 0.032(5) 0.010(4) 0.009(4) 0.002(4) C19 0.075(5) 0.066(5) 0.089(6) 0.013(4) 0.038(5) 0.018(4) C20 0.080(6) 0.075(5) 0.093(6) 0.012(4) 0.039(5) 0.014(4) C21 0.079(6) 0.070(5) 0.095(6) 0.013(4) 0.033(5) 0.020(4) C22 0.079(6) 0.067(5) 0.095(6) 0.015(4) 0.031(5) 0.019(4) C23 0.078(6) 0.069(5) 0.093(6) 0.017(4) 0.033(5) 0.016(4) C24 0.096(8) 0.090(7) 0.185(11) -0.049(8) 0.027(9) 0.011(6) C25 0.088(14) 0.16(2) 0.16(3) -0.03(2) 0.034(16) 0.014(15) C26 0.102(8) 0.094(7) 0.188(11) -0.046(8) 0.025(9) 0.007(6) C27 0.102(8) 0.095(7) 0.189(11) -0.046(8) 0.024(9) 0.009(6) C28 0.100(8) 0.094(7) 0.364(11) -0.063(8) 0.024(9) 0.010(6) N1 0.079(5) 0.073(5) 0.092(5) 0.012(4) 0.038(4) 0.016(4) N2 0.077(5) 0.068(5) 0.093(5) 0.016(4) 0.033(4) 0.017(4) N3 0.098(8) 0.091(7) 0.186(11) -0.047(8) 0.027(9) 0.009(6) N4 0.100(8) 0.093(7) 0.189(11) -0.047(8) 0.024(9) 0.010(6) _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 O6 1.922(8) 7_445 ? Zn1 O9 1.959(8) 4_444 ? Zn1 O7 1.976(8) . ? Zn1 O1 1.982(8) . ? Zn2 O2 1.979(7) . ? Zn2 O14 1.979(9) . ? Zn2 O8 2.013(8) . ? Zn2 O13 2.076(9) . ? Zn2 O10 2.085(8) 4_444 ? Zn3 O12 1.957(9) 2_454 ? Zn3 O11 1.968(8) . ? Zn3 O15 1.973(11) . ? Zn3 O3 1.994(8) 8_455 ? Zn3 O4 2.477(11) 8_455 ? Zn3 C8 2.574(11) 8_455 ? O1 C7 1.255(13) . ? O2 C7 1.259(13) . ? O3 C8 1.265(14) . ? O3 Zn3 1.994(8) 8_556 ? O4 C8 1.288(15) . ? O4 Zn3 2.477(11) 8_556 ? O5 C9 1.216(15) . ? O6 C9 1.273(14) . ? O6 Zn1 1.922(8) 7_445 ? O7 C16 1.271(13) . ? O8 C16 1.253(13) . ? O9 C17 1.266(13) . ? O9 Zn1 1.959(8) 4_454 ? O10 C17 1.290(13) . ? O10 Zn2 2.085(8) 4_454 ? O11 C18 1.272(13) . ? O12 C18 1.266(13) . ? O12 Zn3 1.957(9) 2_454 ? O13 C19 1.23(2) . ? O15 C24 1.26(3) . ? C1 C2 1.379(14) . ? C1 C6 1.387(15) . ? C1 C7 1.513(13) . ? C2 C3 1.409(14) . ? C2 H2A 0.9300 . ? C3 C4 1.407(15) . ? C3 C8 1.476(14) . ? C4 C5 1.397(15) . ? C4 H4A 0.9300 . ? C5 C6 1.414(14) . ? C5 C9 1.525(14) . ? C6 H6A 0.9300 . ? C8 Zn3 2.574(11) 8_556 ? C10 C15 1.400(13) . ? C10 C11 1.420(13) . ? C10 C16 1.495(13) . ? C11 C12 1.388(14) . ? C11 H11A 0.9300 . ? C12 C13 1.392(14) . ? C12 C17 1.501(13) . ? C13 C14 1.401(14) . ? C13 H13A 0.9300 . ? C14 C15 1.387(13) . ? C14 C18 1.513(14) . ? C15 H15A 0.9300 . ? C19 N1 1.36(2) . ? C19 N2 1.41(2) . ? C20 N1 1.44(2) . ? C21 N1 1.46(2) . ? C21 C22 1.50(3) . ? C22 N2 1.45(2) . ? C23 N2 1.43(3) . ? C24 N4 1.29(3) . ? C24 N3 1.36(4) . ? C25 N3 1.51(4) . ? C26 N3 1.35(3) . ? C26 C27 1.61(4) . ? C27 N4 1.39(3) . ? C28 N4 1.52(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 O6 Zn1 O9 113.9(4) 7_445 4_444 ? O6 Zn1 O7 117.4(4) 7_445 . ? O9 Zn1 O7 106.6(4) 4_444 . ? O6 Zn1 O1 93.6(4) 7_445 . ? O9 Zn1 O1 112.7(4) 4_444 . ? O7 Zn1 O1 112.4(4) . . ? O2 Zn2 O14 107.6(4) . . ? O2 Zn2 O8 135.1(4) . . ? O14 Zn2 O8 117.0(4) . . ? O2 Zn2 O13 89.2(4) . . ? O14 Zn2 O13 91.2(5) . . ? O8 Zn2 O13 85.7(4) . . ? O2 Zn2 O10 94.8(4) . 4_444 ? O14 Zn2 O10 89.3(4) . 4_444 ? O8 Zn2 O10 90.2(3) . 4_444 ? O13 Zn2 O10 175.7(4) . 4_444 ? O12 Zn3 O11 124.9(4) 2_454 . ? O12 Zn3 O15 97.8(4) 2_454 . ? O11 Zn3 O15 94.5(5) . . ? O12 Zn3 O3 112.5(4) 2_454 8_455 ? O11 Zn3 O3 115.9(4) . 8_455 ? O15 Zn3 O3 104.4(5) . 8_455 ? O12 Zn3 O4 87.3(4) 2_454 8_455 ? O11 Zn3 O4 96.5(4) . 8_455 ? O15 Zn3 O4 162.3(5) . 8_455 ? O3 Zn3 O4 58.2(3) 8_455 8_455 ? O12 Zn3 C8 100.3(4) 2_454 8_455 ? O11 Zn3 C8 109.4(4) . 8_455 ? O15 Zn3 C8 132.9(5) . 8_455 ? O3 Zn3 C8 28.7(4) 8_455 8_455 ? O4 Zn3 C8 29.5(3) 8_455 8_455 ? C7 O1 Zn1 142.1(7) . . ? C7 O2 Zn2 127.2(7) . . ? C8 O3 Zn3 102.0(7) . 8_556 ? C8 O4 Zn3 79.5(7) . 8_556 ? C9 O6 Zn1 120.2(7) . 7_445 ? C16 O7 Zn1 122.6(7) . . ? C16 O8 Zn2 129.2(7) . . ? C17 O9 Zn1 127.1(7) . 4_454 ? C17 O10 Zn2 131.2(7) . 4_454 ? C18 O11 Zn3 119.8(7) . . ? C18 O12 Zn3 131.3(8) . 2_454 ? C19 O13 Zn2 137.8(12) . . ? C24 O15 Zn3 142.4(17) . . ? C2 C1 C6 120.7(9) . . ? C2 C1 C7 120.5(9) . . ? C6 C1 C7 118.8(9) . . ? C1 C2 C3 120.6(10) . . ? C1 C2 H2A 119.7 . . ? C3 C2 H2A 119.7 . . ? C4 C3 C2 118.6(10) . . ? C4 C3 C8 120.6(10) . . ? C2 C3 C8 120.8(10) . . ? C5 C4 C3 120.9(9) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 C6 118.9(10) . . ? C4 C5 C9 120.7(9) . . ? C6 C5 C9 120.3(10) . . ? C1 C6 C5 120.1(10) . . ? C1 C6 H6A 119.9 . . ? C5 C6 H6A 119.9 . . ? O1 C7 O2 125.8(10) . . ? O1 C7 C1 116.8(9) . . ? O2 C7 C1 117.3(9) . . ? O3 C8 O4 120.2(10) . . ? O3 C8 C3 119.5(10) . . ? O4 C8 C3 120.2(11) . . ? O3 C8 Zn3 49.2(5) . 8_556 ? O4 C8 Zn3 71.1(7) . 8_556 ? C3 C8 Zn3 167.6(9) . 8_556 ? O5 C9 O6 126.9(11) . . ? O5 C9 C5 118.4(11) . . ? O6 C9 C5 114.6(10) . . ? C15 C10 C11 119.5(9) . . ? C15 C10 C16 120.6(9) . . ? C11 C10 C16 119.9(9) . . ? C12 C11 C10 119.3(9) . . ? C12 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? C11 C12 C13 121.0(9) . . ? C11 C12 C17 119.0(9) . . ? C13 C12 C17 120.0(9) . . ? C12 C13 C14 119.5(10) . . ? C12 C13 H13A 120.3 . . ? C14 C13 H13A 120.2 . . ? C15 C14 C13 120.4(10) . . ? C15 C14 C18 118.6(9) . . ? C13 C14 C18 120.9(9) . . ? C14 C15 C10 120.2(9) . . ? C14 C15 H15A 119.9 . . ? C10 C15 H15A 119.9 . . ? O8 C16 O7 125.1(10) . . ? O8 C16 C10 117.4(9) . . ? O7 C16 C10 117.5(9) . . ? O9 C17 O10 125.2(10) . . ? O9 C17 C12 116.5(9) . . ? O10 C17 C12 118.4(9) . . ? O12 C18 O11 125.0(10) . . ? O12 C18 C14 117.7(9) . . ? O11 C18 C14 117.1(9) . . ? O13 C19 N1 128.7(18) . . ? O13 C19 N2 124.6(18) . . ? N1 C19 N2 106.7(15) . . ? N1 C21 C22 103.1(16) . . ? N2 C22 C21 104.4(15) . . ? O15 C24 N4 128(3) . . ? O15 C24 N3 124(3) . . ? N4 C24 N3 108(3) . . ? N3 C26 C27 103(2) . . ? N4 C27 C26 98(2) . . ? C19 N1 C21 112.6(16) . . ? C19 N1 C20 123.4(16) . . ? C21 N1 C20 122.1(17) . . ? C19 N2 C23 125.5(16) . . ? C19 N2 C22 111.0(16) . . ? C23 N2 C22 122.5(16) . . ? C24 N3 C26 112(2) . . ? C24 N3 C25 123(3) . . ? C26 N3 C25 120(3) . . ? C24 N4 C27 115(3) . . ? C24 N4 C28 117(3) . . ? C27 N4 C28 124(2) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.006 -0.038 2127.7 203.5 2 0.500 1.021 0.044 2118.5 201.2 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.39 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.992 _refine_diff_density_min -1.059 _refine_diff_density_rms 0.255 #end