# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Xiang-rong Ha' _publ_contact_author_email haoxr564@nenu.edu.cn _publ_author_name 'Zhong-Min Su' data_1 _database_code_depnum_ccdc_archive 'CCDC 838769' #TrackingRef '- MOF1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Zn2(C9H3O6)(NO3)(C4H9NO)3 _chemical_formula_sum 'C21 H30 N4 O12 Zn2' _chemical_formula_weight 661.23 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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.935(5) _cell_length_b 14.708(5) _cell_length_c 15.359(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 2922.0(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5586 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 1.704 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6695 _exptl_absorpt_correction_T_max 0.6973 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14745 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5143 _reflns_number_gt 4486 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 'SHELXTL and local programs' _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^)+(0.0799P)^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 0.009(15) _refine_ls_number_reflns 5143 _refine_ls_number_parameters 392 _refine_ls_number_restraints 180 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.919 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.001 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 O9 O 0.354(3) 0.146(6) 0.139(5) 0.067(6) Uani 0.446(16) 1 d PD A 1 C18 C 0.4383(12) 0.1359(12) 0.1684(15) 0.082(6) Uani 0.446(16) 1 d PDU A 1 C19 C 0.472(3) 0.0326(17) 0.175(2) 0.124(11) Uani 0.446(16) 1 d PDU A 1 C20 C 0.4808(18) 0.2986(14) 0.1647(17) 0.106(7) Uiso 0.446(16) 1 d PDU A 1 C21 C 0.6099(16) 0.179(3) 0.227(3) 0.131(13) Uani 0.446(16) 1 d PDU A 1 N3 N 0.5089(10) 0.1980(10) 0.1816(10) 0.095(5) Uani 0.446(16) 1 d PDU A 1 O9' O 0.359(2) 0.159(5) 0.125(4) 0.067(6) Uani 0.554(16) 1 d PD A 2 C18' C 0.4422(9) 0.1785(9) 0.1505(9) 0.065(4) Uani 0.554(16) 1 d PDU A 2 C19' C 0.4715(11) 0.2810(9) 0.1342(10) 0.070(4) Uiso 0.554(16) 1 d PDU A 2 C20' C 0.482(3) 0.0262(16) 0.206(2) 0.136(10) Uani 0.554(16) 1 d PDU A 2 C21' C 0.6249(14) 0.151(3) 0.193(2) 0.126(11) Uani 0.554(16) 1 d PDU A 2 N3' N 0.5147(8) 0.1240(8) 0.1785(9) 0.093(4) Uani 0.554(16) 1 d PDU A 2 Zn1 Zn 0.01766(4) 0.02724(3) 0.04707(3) 0.03553(13) Uani 1 1 d . . . Zn2 Zn 0.20196(4) 0.17115(4) 0.16508(3) 0.04246(15) Uani 1 1 d . . . O1 O 0.1305(2) 0.0362(2) -0.0379(2) 0.0501(7) Uani 1 1 d . A . O2 O 0.1680(2) 0.1640(2) 0.0325(2) 0.0487(7) Uani 1 1 d . A . O3 O 0.0568(3) -0.0469(2) 0.1468(2) 0.0501(8) Uani 1 1 d . A . O4 O 0.1967(3) 0.0315(2) 0.1839(2) 0.0570(9) Uani 1 1 d . A . O5 O -0.0613(2) 0.1337(2) 0.0803(2) 0.0480(8) Uani 1 1 d . A . O6 O 0.0419(2) 0.1820(2) 0.18769(19) 0.0484(8) Uani 1 1 d . A . O7 O 0.2502(5) 0.1852(4) 0.2934(3) 0.1074(18) Uani 1 1 d . A . O8 O 0.2114(4) 0.3101(3) 0.1549(4) 0.0982(16) Uani 1 1 d . A . O10 O -0.0828(5) -0.0709(4) 0.0119(4) 0.1042(17) Uani 1 1 d . . . O11 O -0.1024(6) 0.0140(5) -0.0935(5) 0.105(2) Uani 1 1 d . . . O12 O -0.1892(5) -0.1070(5) -0.0900(5) 0.157(3) Uani 1 1 d . . . C1 C 0.2632(3) 0.1293(3) -0.0951(3) 0.0374(9) Uani 1 1 d . A . C2 C 0.3236(3) 0.2072(3) -0.0861(3) 0.0373(9) Uani 1 1 d . . . H2 H 0.3145 0.2454 -0.0384 0.045 Uiso 1 1 calc R . . C3 C 0.3981(3) 0.2277(3) -0.1492(3) 0.0354(9) Uani 1 1 d . . . C4 C 0.4117(3) 0.1700(3) -0.2194(3) 0.0386(9) Uani 1 1 d . . . H4 H 0.4625 0.1827 -0.2605 0.046 Uiso 1 1 calc R . . C5 C 0.3497(3) 0.0929(3) -0.2291(3) 0.0373(9) Uani 1 1 d . . . C6 C 0.2770(3) 0.0734(3) -0.1670(3) 0.0409(9) Uani 1 1 d . . . H6 H 0.2360 0.0218 -0.1732 0.049 Uiso 1 1 calc R . . C7 C 0.1826(3) 0.1084(3) -0.0279(3) 0.0409(10) Uani 1 1 d . . . C8 C 0.1342(3) -0.0306(3) 0.1943(3) 0.0433(10) Uani 1 1 d . . . C9 C -0.0342(3) 0.1896(3) 0.1383(3) 0.0388(10) Uani 1 1 d . . . C10 C 0.2317(6) 0.1870(4) 0.3699(4) 0.0771(18) Uani 1 1 d . . . C11 C 0.1195(9) 0.1812(8) 0.3938(6) 0.148(4) Uani 1 1 d . A . H11A H 0.0792 0.1699 0.3424 0.223 Uiso 1 1 calc R . . H11B H 0.0980 0.2375 0.4197 0.223 Uiso 1 1 calc R . . H11C H 0.1094 0.1325 0.4345 0.223 Uiso 1 1 calc R . . C12 C 0.4035(11) 0.2027(11) 0.4041(9) 0.213(8) Uani 1 1 d . . . H12A H 0.4355 0.1442 0.4098 0.320 Uiso 1 1 calc R A . H12B H 0.4389 0.2458 0.4403 0.320 Uiso 1 1 calc R . . H12C H 0.4070 0.2222 0.3445 0.320 Uiso 1 1 calc R . . C13 C 0.2755(12) 0.1909(9) 0.5246(5) 0.190(7) Uani 1 1 d . . . H13A H 0.2428 0.2458 0.5442 0.285 Uiso 1 1 calc R A . H13B H 0.3402 0.1833 0.5545 0.285 Uiso 1 1 calc R . . H13C H 0.2314 0.1400 0.5368 0.285 Uiso 1 1 calc R . . C14 C 0.1714(6) 0.3786(5) 0.1528(8) 0.115(4) Uani 1 1 d U . . C15 C 0.1162(10) 0.3976(8) 0.0507(10) 0.172(5) Uani 1 1 d . A . H15A H 0.0536 0.4320 0.0575 0.258 Uiso 1 1 calc R . . H15B H 0.1008 0.3404 0.0237 0.258 Uiso 1 1 calc R . . H15C H 0.1638 0.4310 0.0150 0.258 Uiso 1 1 calc R . . C16 C 0.1989(8) 0.4306(7) 0.2710(8) 0.146(4) Uani 1 1 d . . . H16A H 0.2506 0.3841 0.2664 0.219 Uiso 1 1 calc R A . H16B H 0.1470 0.4121 0.3121 0.219 Uiso 1 1 calc R . . H16C H 0.2304 0.4861 0.2905 0.219 Uiso 1 1 calc R . . C17 C 0.0991(8) 0.5316(6) 0.1715(9) 0.165(6) Uani 1 1 d . . . H17A H 0.0563 0.5308 0.1204 0.247 Uiso 1 1 calc R A . H17B H 0.1505 0.5783 0.1657 0.247 Uiso 1 1 calc R . . H17C H 0.0571 0.5437 0.2217 0.247 Uiso 1 1 calc R . . N1 N 0.2940(8) 0.1966(5) 0.4312(4) 0.129(3) Uani 1 1 d . A . N2 N 0.1484(9) 0.4460(8) 0.1813(8) 0.160(4) Uiso 1 1 d U A . N4 N -0.1289(5) -0.0564(4) -0.0539(5) 0.0941(18) 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 O9 0.045(3) 0.066(17) 0.088(18) 0.027(10) 0.011(7) -0.011(3) C18 0.054(10) 0.103(14) 0.091(11) 0.046(10) -0.004(8) -0.018(10) C19 0.153(19) 0.087(15) 0.13(2) 0.079(14) -0.032(17) -0.011(13) C21 0.039(9) 0.16(3) 0.19(3) 0.00(2) -0.019(14) -0.014(12) N3 0.057(8) 0.128(12) 0.100(9) 0.037(9) -0.019(7) -0.014(8) O9' 0.045(3) 0.066(17) 0.088(18) 0.027(10) 0.011(7) -0.011(3) C18' 0.049(7) 0.078(9) 0.068(8) 0.019(7) 0.012(5) -0.014(7) C20' 0.169(19) 0.094(13) 0.15(2) 0.077(13) -0.011(18) 0.014(13) C21' 0.058(10) 0.16(2) 0.16(2) 0.045(18) -0.014(11) -0.019(11) N3' 0.056(6) 0.100(9) 0.123(8) 0.042(7) -0.006(6) 0.004(6) Zn1 0.0425(2) 0.0307(2) 0.0334(2) 0.0023(2) -0.0011(2) 0.00101(19) Zn2 0.0449(3) 0.0400(3) 0.0424(3) -0.0006(2) -0.0062(2) -0.0032(2) O1 0.0541(18) 0.0469(18) 0.0492(18) 0.0005(16) 0.0105(15) -0.0071(15) O2 0.0567(18) 0.0507(18) 0.0388(17) -0.0010(15) 0.0102(14) 0.0027(14) O3 0.0554(18) 0.051(2) 0.0443(18) 0.0162(14) -0.0103(15) 0.0003(14) O4 0.0507(18) 0.0496(19) 0.071(2) 0.0319(17) 0.0031(17) -0.0002(17) O5 0.0552(18) 0.0379(16) 0.0508(19) -0.0098(14) -0.0066(15) 0.0076(14) O6 0.0441(18) 0.062(2) 0.0394(17) -0.0054(15) -0.0061(13) 0.0133(15) O7 0.115(4) 0.145(5) 0.062(3) -0.024(3) -0.033(3) 0.015(4) O8 0.107(4) 0.037(2) 0.151(5) -0.014(2) -0.001(4) -0.014(2) O10 0.106(4) 0.091(4) 0.116(4) -0.002(3) -0.039(3) -0.009(3) O11 0.107(4) 0.092(4) 0.117(4) -0.004(3) -0.038(3) -0.008(3) O12 0.148(6) 0.144(6) 0.180(7) -0.021(5) -0.097(5) -0.068(5) C1 0.041(2) 0.040(2) 0.032(2) -0.0012(18) 0.0028(17) 0.0005(18) C2 0.044(2) 0.033(2) 0.035(2) -0.0090(17) -0.0016(18) 0.0023(17) C3 0.038(2) 0.036(2) 0.033(2) -0.0014(17) -0.0009(17) -0.0015(17) C4 0.040(2) 0.043(2) 0.034(2) -0.0010(19) -0.0011(17) 0.0000(19) C5 0.038(2) 0.035(2) 0.039(2) -0.0056(18) 0.0003(18) 0.0038(17) C6 0.042(2) 0.035(2) 0.045(2) -0.004(2) -0.005(2) -0.0019(17) C7 0.046(2) 0.040(2) 0.037(2) 0.0056(18) -0.0004(18) 0.0016(19) C8 0.045(2) 0.042(2) 0.043(2) 0.008(2) 0.0061(19) 0.008(2) C9 0.043(2) 0.041(2) 0.033(2) 0.0012(18) 0.0041(18) 0.0021(18) C10 0.116(6) 0.058(4) 0.058(4) -0.001(3) -0.021(4) 0.001(3) C11 0.162(10) 0.191(12) 0.092(6) -0.025(7) 0.018(7) -0.039(9) C12 0.152(12) 0.29(2) 0.199(15) -0.009(14) -0.113(11) 0.019(12) C13 0.310(18) 0.194(13) 0.066(5) -0.011(6) -0.051(8) 0.124(13) C14 0.094(5) 0.034(4) 0.218(11) -0.016(5) 0.062(6) -0.010(3) C15 0.136(9) 0.159(11) 0.222(14) 0.072(11) -0.005(10) -0.018(8) C16 0.120(7) 0.119(8) 0.198(11) -0.018(8) 0.060(8) -0.044(7) C17 0.148(9) 0.075(6) 0.271(15) 0.039(8) 0.105(10) 0.045(6) N1 0.211(9) 0.098(5) 0.077(4) -0.030(3) -0.080(5) 0.056(5) N4 0.091(4) 0.073(4) 0.119(5) -0.011(4) -0.046(4) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O9 C18 1.18(2) . ? O9 Zn2 2.05(6) . ? C18 N3 1.308(14) . ? C18 C19 1.58(2) . ? C20 N3 1.54(2) . ? C21 N3 1.50(2) . ? O9' C18' 1.183(19) . ? O9' Zn2 2.13(5) . ? C18' N3' 1.307(13) . ? C18' C19' 1.575(18) . ? C20' N3' 1.56(2) . ? C21' N3' 1.494(19) . ? Zn1 O5 1.938(3) . ? Zn1 O3 1.947(3) . ? Zn1 O1 1.962(3) . ? Zn1 O10 2.016(5) . ? Zn2 O8 2.054(4) . ? Zn2 O4 2.076(3) . ? Zn2 O7 2.078(4) . ? Zn2 O2 2.085(3) . ? Zn2 O6 2.106(3) . ? O1 C7 1.266(5) . ? O2 C7 1.251(5) . ? O3 C8 1.262(6) . ? O4 C8 1.230(6) . ? O5 C9 1.262(5) . ? O6 C9 1.248(5) . ? O7 C10 1.198(8) . ? O8 C14 1.132(8) . ? O10 N4 1.193(7) . ? O11 N4 1.249(9) . ? O12 N4 1.212(7) . ? C1 C6 1.389(6) . ? C1 C2 1.393(6) . ? C1 C7 1.500(6) . ? C2 C3 1.399(6) . ? C2 H2 0.9300 . ? C3 C4 1.383(6) . ? C3 C9 1.508(6) 3 ? C4 C5 1.397(6) . ? C4 H4 0.9300 . ? C5 C6 1.369(6) . ? C5 C8 1.506(6) 2_554 ? C6 H6 0.9300 . ? C8 C5 1.506(6) 2 ? C9 C3 1.508(6) 3_455 ? C10 N1 1.248(9) . ? C10 C11 1.500(13) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N1 1.478(16) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N1 1.457(12) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N2 1.123(13) . ? C14 C15 1.746(17) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N2 1.541(15) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N2 1.421(13) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 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 C18 O9 Zn2 147(7) . . ? O9 C18 N3 128(4) . . ? O9 C18 C19 113(4) . . ? N3 C18 C19 118.1(18) . . ? C18 N3 C21 123(2) . . ? C18 N3 C20 118.6(14) . . ? C21 N3 C20 117(2) . . ? C18' O9' Zn2 138(6) . . ? O9' C18' N3' 128(4) . . ? O9' C18' C19' 114(3) . . ? N3' C18' C19' 117.8(11) . . ? C18' N3' C21' 124.8(17) . . ? C18' N3' C20' 117.6(15) . . ? C21' N3' C20' 117(2) . . ? O5 Zn1 O3 112.48(14) . . ? O5 Zn1 O1 120.85(14) . . ? O3 Zn1 O1 111.57(14) . . ? O5 Zn1 O10 108.0(2) . . ? O3 Zn1 O10 88.70(19) . . ? O1 Zn1 O10 110.45(19) . . ? O8 Zn2 O4 176.08(18) . . ? O8 Zn2 O7 87.4(2) . . ? O4 Zn2 O7 88.7(2) . . ? O8 Zn2 O2 89.36(19) . . ? O4 Zn2 O2 94.50(14) . . ? O7 Zn2 O2 173.9(2) . . ? O8 Zn2 O9 96(2) . . ? O4 Zn2 O9 83(2) . . ? O7 Zn2 O9 85(2) . . ? O2 Zn2 O9 90(2) . . ? O8 Zn2 O9' 90.4(18) . . ? O4 Zn2 O9' 89.3(18) . . ? O7 Zn2 O9' 90.0(15) . . ? O2 Zn2 O9' 84.9(15) . . ? O9 Zn2 O9' 8(3) . . ? O8 Zn2 O6 89.74(18) . . ? O4 Zn2 O6 91.12(13) . . ? O7 Zn2 O6 97.54(19) . . ? O2 Zn2 O6 87.57(12) . . ? O9 Zn2 O6 174(3) . . ? O9' Zn2 O6 172.5(15) . . ? C7 O1 Zn1 111.8(3) . . ? C7 O2 Zn2 136.5(3) . . ? C8 O3 Zn1 123.7(3) . . ? C8 O4 Zn2 140.7(3) . . ? C9 O5 Zn1 124.5(3) . . ? C9 O6 Zn2 133.0(3) . . ? C10 O7 Zn2 150.7(6) . . ? C14 O8 Zn2 149.4(5) . . ? N4 O10 Zn1 115.0(5) . . ? C6 C1 C2 119.6(4) . . ? C6 C1 C7 121.0(4) . . ? C2 C1 C7 119.4(4) . . ? C1 C2 C3 119.6(4) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 119.7(4) . . ? C4 C3 C9 120.5(4) . 3 ? C2 C3 C9 119.8(4) . 3 ? C3 C4 C5 120.5(4) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 119.4(4) . . ? C6 C5 C8 120.8(4) . 2_554 ? C4 C5 C8 119.8(4) . 2_554 ? C5 C6 C1 121.2(4) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? O2 C7 O1 123.8(4) . . ? O2 C7 C1 118.8(4) . . ? O1 C7 C1 117.4(4) . . ? O4 C8 O3 126.0(4) . . ? O4 C8 C5 117.5(4) . 2 ? O3 C8 C5 116.5(4) . 2 ? O6 C9 O5 126.1(4) . . ? O6 C9 C3 117.6(4) . 3_455 ? O5 C9 C3 116.3(4) . 3_455 ? O7 C10 N1 127.9(9) . . ? O7 C10 C11 115.5(7) . . ? N1 C10 C11 116.5(8) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 H13A 109.5 . . ? N1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 O8 153.5(15) . . ? N2 C14 C15 95.7(10) . . ? O8 C14 C15 110.8(9) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C10 N1 C13 129.1(12) . . ? C10 N1 C12 114.3(8) . . ? C13 N1 C12 116.0(9) . . ? C14 N2 C17 149.4(15) . . ? C14 N2 C16 96.1(12) . . ? C17 N2 C16 114.5(11) . . ? O10 N4 O12 126.8(8) . . ? O10 N4 O11 115.0(7) . . ? O12 N4 O11 117.7(8) . . ? 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 Zn2 O9 C18 N3 -91(9) . . . . ? Zn2 O9 C18 C19 101(11) . . . . ? O9 C18 N3 C21 174(6) . . . . ? C19 C18 N3 C21 -18(4) . . . . ? O9 C18 N3 C20 5(7) . . . . ? C19 C18 N3 C20 173(2) . . . . ? Zn2 O9' C18' N3' 110(6) . . . . ? Zn2 O9' C18' C19' -80(5) . . . . ? O9' C18' N3' C21' 167(5) . . . . ? C19' C18' N3' C21' -3(3) . . . . ? O9' C18' N3' C20' -19(5) . . . . ? C19' C18' N3' C20' 172.1(17) . . . . ? C18 O9 Zn2 O8 91(10) . . . . ? C18 O9 Zn2 O4 -85(10) . . . . ? C18 O9 Zn2 O7 4(10) . . . . ? C18 O9 Zn2 O2 -180(11) . . . . ? C18 O9 Zn2 O6 -109(20) . . . . ? C18' O9' Zn2 O8 65(5) . . . . ? C18' O9' Zn2 O4 -111(5) . . . . ? C18' O9' Zn2 O7 -22(5) . . . . ? C18' O9' Zn2 O2 155(6) . . . . ? C18' O9' Zn2 O9 -73(31) . . . . ? C18' O9' Zn2 O6 156(9) . . . . ? O5 Zn1 O1 C7 39.0(3) . . . . ? O3 Zn1 O1 C7 -96.6(3) . . . . ? O10 Zn1 O1 C7 166.4(3) . . . . ? O8 Zn2 O2 C7 149.6(4) . . . . ? O4 Zn2 O2 C7 -29.7(4) . . . . ? O7 Zn2 O2 C7 92(2) . . . . ? O9 Zn2 O2 C7 53(2) . . . . ? O9' Zn2 O2 C7 59.1(19) . . . . ? O6 Zn2 O2 C7 -120.7(4) . . . . ? O5 Zn1 O3 C8 -82.5(4) . . . . ? O1 Zn1 O3 C8 57.0(4) . . . . ? O10 Zn1 O3 C8 168.5(4) . . . . ? O8 Zn2 O4 C8 110(3) . . . . ? O7 Zn2 O4 C8 105.1(5) . . . . ? O2 Zn2 O4 C8 -80.0(5) . . . . ? O9 Zn2 O4 C8 -170(2) . . . . ? O9' Zn2 O4 C8 -164.9(16) . . . . ? O6 Zn2 O4 C8 7.6(5) . . . . ? O3 Zn1 O5 C9 51.1(4) . . . . ? O1 Zn1 O5 C9 -84.1(4) . . . . ? O10 Zn1 O5 C9 147.4(4) . . . . ? O8 Zn2 O6 C9 83.2(4) . . . . ? O4 Zn2 O6 C9 -100.6(4) . . . . ? O7 Zn2 O6 C9 170.6(4) . . . . ? O2 Zn2 O6 C9 -6.2(4) . . . . ? O9 Zn2 O6 C9 -77(16) . . . . ? O9' Zn2 O6 C9 -8(14) . . . . ? O8 Zn2 O7 C10 102.3(12) . . . . ? O4 Zn2 O7 C10 -78.1(12) . . . . ? O2 Zn2 O7 C10 160.4(14) . . . . ? O9 Zn2 O7 C10 -161(3) . . . . ? O9' Zn2 O7 C10 -167(2) . . . . ? O6 Zn2 O7 C10 12.9(12) . . . . ? O4 Zn2 O8 C14 -108(3) . . . . ? O7 Zn2 O8 C14 -102.9(15) . . . . ? O2 Zn2 O8 C14 82.2(15) . . . . ? O9 Zn2 O8 C14 172(3) . . . . ? O9' Zn2 O8 C14 167(2) . . . . ? O6 Zn2 O8 C14 -5.3(15) . . . . ? O5 Zn1 O10 N4 68.6(6) . . . . ? O3 Zn1 O10 N4 -178.2(6) . . . . ? O1 Zn1 O10 N4 -65.6(6) . . . . ? C6 C1 C2 C3 -0.6(6) . . . . ? C7 C1 C2 C3 -179.2(4) . . . . ? C1 C2 C3 C4 -0.6(6) . . . . ? C1 C2 C3 C9 -178.2(4) . . . 3 ? C2 C3 C4 C5 1.8(6) . . . . ? C9 C3 C4 C5 179.4(4) 3 . . . ? C3 C4 C5 C6 -1.7(6) . . . . ? C3 C4 C5 C8 -179.7(4) . . . 2_554 ? C4 C5 C6 C1 0.5(6) . . . . ? C8 C5 C6 C1 178.5(4) 2_554 . . . ? C2 C1 C6 C5 0.7(6) . . . . ? C7 C1 C6 C5 179.2(4) . . . . ? Zn2 O2 C7 O1 76.7(6) . . . . ? Zn2 O2 C7 C1 -105.9(4) . . . . ? Zn1 O1 C7 O2 4.5(5) . . . . ? Zn1 O1 C7 C1 -172.9(3) . . . . ? C6 C1 C7 O2 -175.1(4) . . . . ? C2 C1 C7 O2 3.5(6) . . . . ? C6 C1 C7 O1 2.5(6) . . . . ? C2 C1 C7 O1 -178.9(4) . . . . ? Zn2 O4 C8 O3 51.3(8) . . . . ? Zn2 O4 C8 C5 -128.4(4) . . . 2 ? Zn1 O3 C8 O4 -2.1(7) . . . . ? Zn1 O3 C8 C5 177.5(3) . . . 2 ? Zn2 O6 C9 O5 60.2(6) . . . . ? Zn2 O6 C9 C3 -121.1(4) . . . 3_455 ? Zn1 O5 C9 O6 -6.2(6) . . . . ? Zn1 O5 C9 C3 175.0(3) . . . 3_455 ? Zn2 O7 C10 N1 177.8(8) . . . . ? Zn2 O7 C10 C11 -5.4(16) . . . . ? Zn2 O8 C14 N2 106(2) . . . . ? Zn2 O8 C14 C15 -77.7(15) . . . . ? O7 C10 N1 C13 -173.9(9) . . . . ? C11 C10 N1 C13 9.3(13) . . . . ? O7 C10 N1 C12 -2.6(14) . . . . ? C11 C10 N1 C12 -179.4(10) . . . . ? O8 C14 N2 C17 176.2(15) . . . . ? C15 C14 N2 C17 0(2) . . . . ? O8 C14 N2 C16 -2(2) . . . . ? C15 C14 N2 C16 -178.9(7) . . . . ? Zn1 O10 N4 O12 176.2(7) . . . . ? Zn1 O10 N4 O11 4.8(10) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.610 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.073 data_2 _database_code_depnum_ccdc_archive 'CCDC 838770' #TrackingRef '- MOF1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Zn11(C9H3O6)6(NO3)4(C6H13NO)9 _chemical_formula_sum 'C108 H135 N13 O57 Zn11' _chemical_formula_weight 3246.36 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 Cubic _symmetry_space_group_name_H-M 'P m -3 m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' 'z, x, y' 'y, z, x' '-z, -x, y' '-y, z, -x' 'z, -x, -y' '-y, -z, x' '-z, x, -y' 'y, -z, -x' '-y, -x, -z' 'y, x, -z' 'y, -x, z' '-y, x, z' '-x, -z, -y' '-z, -y, -x' 'x, z, -y' '-z, y, x' 'x, -z, y' 'z, y, -x' '-x, z, y' 'z, -y, x' '-x, -y, -z' 'x, y, -z' '-x, y, z' 'x, -y, z' '-z, -x, -y' '-y, -z, -x' 'z, x, -y' 'y, -z, x' '-z, x, y' 'y, z, -x' 'z, -x, y' '-y, z, x' 'y, x, z' '-y, -x, z' '-y, x, -z' 'y, -x, -z' 'x, z, y' 'z, y, x' '-x, -z, y' 'z, -y, -x' '-x, z, -y' '-z, -y, x' 'x, -z, -y' '-z, y, -x' _cell_length_a 20.573(5) _cell_length_b 20.573(5) _cell_length_c 20.573(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 8707(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2586 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 0.780 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8410 _exptl_absorpt_correction_T_max 0.8534 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 44723 _diffrn_reflns_av_R_equivalents 0.1422 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 24.98 _reflns_number_total 1582 _reflns_number_gt 880 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 'SHELXTL and local programs' _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^)+(0.2114P)^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 1582 _refine_ls_number_parameters 67 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.1762 _refine_ls_R_factor_gt 0.1016 _refine_ls_wR_factor_ref 0.3583 _refine_ls_wR_factor_gt 0.2972 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3600(8) 1.0000 0.3600(8) 0.092(6) Uani 1 4 d SU . . C2 C 0.3341(5) 0.9410(7) 0.3341(5) 0.088(4) Uani 1 2 d SU . . H2 H 0.3491 0.9011 0.3491 0.105 Uiso 1 2 calc SR . . C3 C 0.2882(4) 0.9430(7) 0.2882(4) 0.085(4) Uani 1 2 d SU . . C4 C 0.2651(7) 1.0000 0.2651(7) 0.090(6) Uani 1 4 d SU . . H4 H 0.2331 1.0000 0.2331 0.108 Uiso 1 4 calc SR . . C5 C 0.4133(6) 1.0000 0.4133(6) 0.087(6) Uani 1 4 d SU . . C6 C 0.2610(6) 0.8812(9) 0.2610(6) 0.117(5) Uani 1 2 d SU . . O1 O 0.4318(3) 1.0539(5) 0.4318(3) 0.096(3) Uani 1 2 d SU . . O2 O 0.2831(3) 0.8283(5) 0.2831(3) 0.104(3) Uani 1 2 d SU . . O3 O 0.2186(4) 0.8877(6) 0.2186(4) 0.164(6) Uani 1 2 d SU . . O4 O 0.5000 1.1712(10) 0.5000 0.121(8) Uani 1 8 d SU . . O5? O 0.3249(3) 0.6751(3) 0.3249(3) 0.086(5) Uani 1 6 d SU . . O6? O 0.1088(6) 0.8912(6) 0.1088(6) 0.192(11) Uani 1 6 d SU . . Zn1 Zn 0.5000 1.07243(12) 0.5000 0.0723(10) Uani 1 8 d SU . . Zn2 Zn 0.26319(8) 0.73681(8) 0.26319(8) 0.0843(11) Uani 1 6 d SU . . Zn3 Zn 0.16524(8) 0.83476(8) 0.16524(8) 0.0974(12) Uani 1 6 d SU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.087(9) 0.100(15) 0.087(9) 0.000 0.018(11) 0.000 C2 0.096(6) 0.073(8) 0.096(6) -0.008(6) 0.029(9) -0.008(6) C3 0.080(5) 0.094(10) 0.080(5) -0.016(5) -0.034(8) -0.016(5) C4 0.082(8) 0.106(16) 0.082(8) 0.000 -0.015(11) 0.000 C5 0.058(7) 0.14(2) 0.058(7) 0.000 -0.017(9) 0.000 C6 0.119(8) 0.113(12) 0.119(8) -0.007(7) -0.045(10) -0.007(7) O1 0.094(5) 0.100(7) 0.094(5) -0.014(4) -0.032(6) -0.014(4) O2 0.109(5) 0.093(7) 0.109(5) -0.010(4) -0.021(6) -0.010(4) O3 0.193(9) 0.106(9) 0.193(9) -0.027(5) -0.098(11) -0.027(5) O4 0.137(11) 0.088(14) 0.137(11) 0.000 0.000 0.000 O5? 0.086(5) 0.086(5) 0.086(5) 0.042(4) -0.042(4) 0.042(4) O6? 0.192(11) 0.192(11) 0.192(11) 0.063(9) -0.063(9) 0.063(9) Zn1 0.0896(15) 0.0377(14) 0.0896(15) 0.000 0.000 0.000 Zn2 0.0843(11) 0.0843(11) 0.0843(11) 0.0017(9) -0.0017(9) 0.0017(9) Zn3 0.0974(12) 0.0974(12) 0.0974(12) 0.0096(9) -0.0096(9) 0.0096(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.430(17) . ? C1 C2 1.430(17) 28_575 ? C1 C5 1.55(3) . ? C2 C3 1.335(18) . ? C2 H2 0.9300 . ? C3 C4 1.351(16) . ? C3 C6 1.50(2) . ? C4 C3 1.351(16) 28_575 ? C4 H4 0.9300 . ? C5 O1 1.234(11) . ? C5 O1 1.234(11) 28_575 ? C6 O3 1.242(19) . ? C6 O2 1.26(2) . ? O1 Zn1 2.019(9) . ? O2 Zn2 1.969(11) . ? O3 Zn3 1.896(11) . ? O4 Zn1 2.03(2) . ? O5? Zn2 2.200(11) . ? O6? Zn3 2.01(2) . ? Zn1 O1 2.019(9) 4_656 ? Zn1 O1 2.019(9) 26_556 ? Zn1 O1 2.019(9) 27_655 ? Zn1 Zn1 2.980(5) 25_676 ? Zn2 O2 1.969(11) 9_566 ? Zn2 O2 1.969(11) 10_665 ? Zn3 O3 1.896(11) 10_665 ? Zn3 O3 1.896(11) 9_566 ? 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 C2 C1 C2 116(2) . 28_575 ? C2 C1 C5 121.9(10) . . ? C2 C1 C5 121.9(10) 28_575 . ? C3 C2 C1 120.1(15) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 121.6(15) . . ? C2 C3 C6 120.0(15) . . ? C4 C3 C6 118.3(14) . . ? C3 C4 C3 120.4(19) 28_575 . ? C3 C4 H4 119.8 28_575 . ? C3 C4 H4 119.8 . . ? O1 C5 O1 128.1(18) . 28_575 ? O1 C5 C1 115.9(9) . . ? O1 C5 C1 115.9(9) 28_575 . ? O3 C6 O2 126.8(17) . . ? O3 C6 C3 115.6(17) . . ? O2 C6 C3 117.6(15) . . ? C5 O1 Zn1 126.8(11) . . ? C6 O2 Zn2 132.4(11) . . ? C6 O3 Zn3 138.7(13) . . ? O1 Zn1 O1 158.3(6) . 4_656 ? O1 Zn1 O1 87.97(11) . 26_556 ? O1 Zn1 O1 87.97(11) 4_656 26_556 ? O1 Zn1 O1 87.97(11) . 27_655 ? O1 Zn1 O1 87.97(11) 4_656 27_655 ? O1 Zn1 O1 158.3(6) 26_556 27_655 ? O1 Zn1 O4 100.9(3) . . ? O1 Zn1 O4 100.9(3) 4_656 . ? O1 Zn1 O4 100.9(3) 26_556 . ? O1 Zn1 O4 100.9(3) 27_655 . ? O1 Zn1 Zn1 79.1(3) . 25_676 ? O1 Zn1 Zn1 79.1(3) 4_656 25_676 ? O1 Zn1 Zn1 79.1(3) 26_556 25_676 ? O1 Zn1 Zn1 79.1(3) 27_655 25_676 ? O4 Zn1 Zn1 180.000(3) . 25_676 ? O2 Zn2 O2 110.7(3) . 9_566 ? O2 Zn2 O2 110.7(3) . 10_665 ? O2 Zn2 O2 110.7(3) 9_566 10_665 ? O2 Zn2 O5? 108.2(3) . . ? O2 Zn2 O5? 108.2(3) 9_566 . ? O2 Zn2 O5? 108.2(3) 10_665 . ? O3 Zn3 O3 109.3(4) . 10_665 ? O3 Zn3 O3 109.3(4) . 9_566 ? O3 Zn3 O3 109.3(4) 10_665 9_566 ? O3 Zn3 O6? 109.6(4) . . ? O3 Zn3 O6? 109.6(4) 10_665 . ? O3 Zn3 O6? 109.6(4) 9_566 . ? 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 C2 C1 C2 C3 0.000(6) 28_575 . . . ? C5 C1 C2 C3 180.000(4) . . . . ? C1 C2 C3 C4 0.000(6) . . . . ? C1 C2 C3 C6 180.000(4) . . . . ? C2 C3 C4 C3 0.000(7) . . . 28_575 ? C6 C3 C4 C3 180.000(4) . . . 28_575 ? C2 C1 C5 O1 180.000(3) . . . . ? C2 C1 C5 O1 0.000(6) 28_575 . . . ? C2 C1 C5 O1 0.000(6) . . . 28_575 ? C2 C1 C5 O1 180.000(3) 28_575 . . 28_575 ? C2 C3 C6 O3 180.000(4) . . . . ? C4 C3 C6 O3 0.000(6) . . . . ? C2 C3 C6 O2 0.000(5) . . . . ? C4 C3 C6 O2 180.000(4) . . . . ? O1 C5 O1 Zn1 0.000(6) 28_575 . . . ? C1 C5 O1 Zn1 180.000(2) . . . . ? O3 C6 O2 Zn2 0.000(6) . . . . ? C3 C6 O2 Zn2 180.000(4) . . . . ? O2 C6 O3 Zn3 0.000(8) . . . . ? C3 C6 O3 Zn3 180.000(3) . . . . ? C5 O1 Zn1 O1 0.000(3) . . . 4_656 ? C5 O1 Zn1 O1 -79.3(3) . . . 26_556 ? C5 O1 Zn1 O1 79.3(3) . . . 27_655 ? C5 O1 Zn1 O4 180.000(4) . . . . ? C5 O1 Zn1 Zn1 0.000(3) . . . 25_676 ? C6 O2 Zn2 O2 61.6(4) . . . 9_566 ? C6 O2 Zn2 O2 -61.6(4) . . . 10_665 ? C6 O2 Zn2 O5? 180.000(3) . . . . ? C6 O3 Zn3 O3 59.8(5) . . . 10_665 ? C6 O3 Zn3 O3 -59.8(5) . . . 9_566 ? C6 O3 Zn3 O6? 180.000(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.248 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.118 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 _platon_squeeze_void_content 1 -0.022 -0.009 -0.007 5951 1474 ' ' _platon_squeeze_details ; ; data_3 _database_code_depnum_ccdc_archive 'CCDC 838771' #TrackingRef '- MOF1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety Zn11(C9H3O6)6(NO3)4(C7H15NO)8 _chemical_formula_sum 'C110 H138 N12 O56 Zn11' _chemical_formula_weight 3243.39 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 Cubic _symmetry_space_group_name_H-M 'P m -3 m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' _cell_length_a 20.6155(7) _cell_length_b 20.6155(7) _cell_length_c 20.6155(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8761.6(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2586 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 0.775 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8432 _exptl_absorpt_correction_T_max 0.8481 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 44794 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1591 _reflns_number_gt 1119 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 'SHELXTL and local programs' _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^)+(0.1830P)^2^+0.1741P] 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 1591 _refine_ls_number_parameters 67 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.2702 _refine_ls_wR_factor_gt 0.2512 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 0.0000 0.42776(8) 0.0000 0.0794(7) Uani 1 8 d S . . Zn2 Zn 0.23888(4) 0.23888(4) 0.23888(4) 0.0693(6) Uani 1 6 d S . . Zn3 Zn 0.33549(5) 0.33549(5) 0.33549(5) 0.0977(8) Uani 1 6 d S . . O1 O 0.0689(2) 0.4458(3) 0.0689(2) 0.0987(19) Uani 1 2 d S . . O2 O 0.2157(2) 0.3279(3) 0.2157(2) 0.100(2) Uani 1 2 d S . . O3 O 0.2832(3) 0.3868(4) 0.2832(3) 0.144(3) Uani 1 2 d S . . O4 O 0.0000 0.3329(5) 0.0000 0.105(4) Uani 1 8 d S . . O5? O 0.3884(5) 0.3884(5) 0.3884(5) 0.333(19) Uani 1 6 d S . . O6? O 0.1772(4) 0.1772(4) 0.1772(4) 0.144(5) Uani 1 6 d S . . C1 C 0.0894(5) 0.5000 0.0894(5) 0.090(3) Uani 1 4 d S . . C2 C 0.1400(4) 0.5000 0.1400(4) 0.074(3) Uani 1 4 d S . . C3 C 0.1638(3) 0.4415(4) 0.1638(3) 0.078(2) Uani 1 2 d S . . H3 H 0.1481 0.4022 0.1481 0.093 Uiso 1 2 calc SR . . C4 C 0.2103(3) 0.4427(4) 0.2103(3) 0.082(2) Uani 1 2 d S . . C5 C 0.2339(4) 0.5000 0.2339(4) 0.081(3) Uani 1 4 d S . . H5 H 0.2658 0.5000 0.2658 0.097 Uiso 1 4 calc SR . . C6 C 0.2394(4) 0.3801(5) 0.2394(4) 0.095(3) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0986(10) 0.0410(9) 0.0986(10) 0.000 0.000 0.000 Zn2 0.0693(6) 0.0693(6) 0.0693(6) -0.0018(4) -0.0018(4) -0.0018(4) Zn3 0.0977(8) 0.0977(8) 0.0977(8) -0.0132(5) -0.0132(5) -0.0132(5) O1 0.110(3) 0.077(4) 0.110(3) -0.006(2) -0.018(4) -0.006(2) O2 0.119(3) 0.064(3) 0.119(3) 0.003(2) -0.007(4) 0.003(2) O3 0.167(5) 0.098(5) 0.167(5) 0.013(3) -0.068(7) 0.013(3) O4 0.131(7) 0.052(6) 0.131(7) 0.000 0.000 0.000 O5? 0.333(19) 0.333(19) 0.333(19) -0.128(12) -0.128(12) -0.128(12) O6? 0.144(5) 0.144(5) 0.144(5) -0.026(5) -0.026(5) -0.026(5) C1 0.098(6) 0.073(8) 0.098(6) 0.000 0.006(7) 0.000 C2 0.083(5) 0.058(6) 0.083(5) 0.000 0.009(6) 0.000 C3 0.086(3) 0.062(5) 0.086(3) -0.007(3) 0.011(4) -0.007(3) C4 0.093(3) 0.061(5) 0.093(3) 0.009(3) 0.001(5) 0.009(3) C5 0.094(5) 0.055(6) 0.094(5) 0.000 0.001(7) 0.000 C6 0.104(4) 0.077(6) 0.104(4) 0.007(4) 0.018(6) 0.007(4) _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 1.956(11) . ? Zn1 O1 2.042(6) . ? Zn1 O1 2.042(6) 3 ? Zn1 O1 2.042(6) 28 ? Zn1 O1 2.042(6) 26 ? Zn1 Zn1 2.979(3) 25_565 ? Zn2 O2 1.956(6) 5 ? Zn2 O2 1.956(6) . ? Zn2 O2 1.956(6) 9 ? Zn2 O6? 2.201(14) . ? Zn3 O3 1.856(7) 5 ? Zn3 O3 1.856(7) . ? Zn3 O3 1.856(7) 9 ? Zn3 O5? 1.889(18) . ? O1 C1 1.268(8) . ? O2 C6 1.280(12) . ? O3 C6 1.285(12) . ? C1 O1 1.268(8) 27_565 ? C1 C2 1.477(18) . ? C2 C3 1.392(11) 27_565 ? C2 C3 1.392(11) . ? C3 C4 1.356(12) . ? C3 H3 0.9300 . ? C4 C5 1.367(11) . ? C4 C6 1.544(12) . ? C5 C4 1.367(11) 27_565 ? C5 H5 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 O4 Zn1 O1 100.47(18) . . ? O4 Zn1 O1 100.47(18) . 3 ? O1 Zn1 O1 159.1(4) . 3 ? O4 Zn1 O1 100.47(18) . 28 ? O1 Zn1 O1 88.11(6) . 28 ? O1 Zn1 O1 88.11(6) 3 28 ? O4 Zn1 O1 100.47(18) . 26 ? O1 Zn1 O1 88.11(6) . 26 ? O1 Zn1 O1 88.11(6) 3 26 ? O1 Zn1 O1 159.1(4) 28 26 ? O4 Zn1 Zn1 180.0 . 25_565 ? O1 Zn1 Zn1 79.53(18) . 25_565 ? O1 Zn1 Zn1 79.53(18) 3 25_565 ? O1 Zn1 Zn1 79.53(18) 28 25_565 ? O1 Zn1 Zn1 79.53(18) 26 25_565 ? O2 Zn2 O2 113.53(17) 5 . ? O2 Zn2 O2 113.53(17) 5 9 ? O2 Zn2 O2 113.53(17) . 9 ? O2 Zn2 O6? 105.0(2) 5 . ? O2 Zn2 O6? 105.0(2) . . ? O2 Zn2 O6? 105.0(2) 9 . ? O3 Zn3 O3 109.0(3) 5 . ? O3 Zn3 O3 109.0(3) 5 9 ? O3 Zn3 O3 109.0(3) . 9 ? O3 Zn3 O5? 109.9(3) 5 . ? O3 Zn3 O5? 109.9(3) . . ? O3 Zn3 O5? 109.9(3) 9 . ? C1 O1 Zn1 128.6(7) . . ? C6 O2 Zn2 127.0(7) . . ? C6 O3 Zn3 139.0(7) . . ? O1 C1 O1 123.8(13) . 27_565 ? O1 C1 C2 118.1(6) . . ? O1 C1 C2 118.1(6) 27_565 . ? C3 C2 C3 120.3(11) 27_565 . ? C3 C2 C1 119.8(6) 27_565 . ? C3 C2 C1 119.8(6) . . ? C4 C3 C2 118.7(8) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 121.3(8) . . ? C3 C4 C6 122.2(8) . . ? C5 C4 C6 116.4(9) . . ? C4 C5 C4 119.5(12) . 27_565 ? C4 C5 H5 120.2 . . ? C4 C5 H5 120.2 27_565 . ? O2 C6 O3 128.9(9) . . ? O2 C6 C4 113.9(9) . . ? O3 C6 C4 117.2(9) . . ? 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 O4 Zn1 O1 C1 180.0 . . . . ? O1 Zn1 O1 C1 0.000(1) 3 . . . ? O1 Zn1 O1 C1 -79.70(17) 28 . . . ? O1 Zn1 O1 C1 79.70(17) 26 . . . ? Zn1 Zn1 O1 C1 0.0 25_565 . . . ? O2 Zn2 O2 C6 65.8(3) 5 . . . ? O2 Zn2 O2 C6 -65.8(3) 9 . . . ? O6? Zn2 O2 C6 180.000(1) . . . . ? O3 Zn3 O3 C6 -59.4(3) 5 . . . ? O3 Zn3 O3 C6 59.4(3) 9 . . . ? O5? Zn3 O3 C6 180.000(2) . . . . ? Zn1 O1 C1 O1 0.000(2) . . . 27_565 ? Zn1 O1 C1 C2 180.000(1) . . . . ? O1 C1 C2 C3 180.000(2) . . . 27_565 ? O1 C1 C2 C3 0.000(2) 27_565 . . 27_565 ? O1 C1 C2 C3 0.000(2) . . . . ? O1 C1 C2 C3 180.000(2) 27_565 . . . ? C3 C2 C3 C4 0.000(2) 27_565 . . . ? C1 C2 C3 C4 180.000(2) . . . . ? C2 C3 C4 C5 0.000(2) . . . . ? C2 C3 C4 C6 180.000(1) . . . . ? C3 C4 C5 C4 0.000(2) . . . 27_565 ? C6 C4 C5 C4 180.0 . . . 27_565 ? Zn2 O2 C6 O3 0.000(2) . . . . ? Zn2 O2 C6 C4 180.000(1) . . . . ? Zn3 O3 C6 O2 0.000(3) . . . . ? Zn3 O3 C6 C4 180.000(1) . . . . ? C3 C4 C6 O2 0.000(2) . . . . ? C5 C4 C6 O2 180.000(2) . . . . ? C3 C4 C6 O3 180.000(2) . . . . ? C5 C4 C6 O3 0.000(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.286 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.104 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 _platon_squeeze_void_content 1 -0.019 -0.011 -0.010 6012 1573 ' ' _platon_squeeze_details ; ; data_4 _database_code_depnum_ccdc_archive 'CCDC 838772' #TrackingRef '- MOF1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H3 O6 Zn, C4 H9 N O , C2 H8 N ' _chemical_formula_sum 'C15 H20 N2 O7 Zn' _chemical_formula_weight 405.70 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 'P 21/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 9.320(5) _cell_length_b 16.107(5) _cell_length_c 12.608(5) _cell_angle_alpha 90.000 _cell_angle_beta 100.942(5) _cell_angle_gamma 90.000 _cell_volume 1858.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2586 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 1.359 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7634 _exptl_absorpt_correction_T_max 0.8140 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9299 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0761 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.06 _reflns_number_total 3281 _reflns_number_gt 2185 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 'SHELXTL and local programs' _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^)+(0.0681P)^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 3281 _refine_ls_number_parameters 283 _refine_ls_number_restraints 231 _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1269 _refine_ls_wR_factor_gt 0.1101 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.944 _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 O7 O 0.349(2) 0.0913(17) 0.393(3) 0.141(9) Uani 0.59(2) 1 d PDU A 1 C12 C 0.496(2) 0.0863(13) 0.4106(13) 0.116(7) Uani 0.59(2) 1 d PDU A 1 C13 C 0.571(3) 0.0384(16) 0.3318(16) 0.126(8) Uani 0.59(2) 1 d PDU A 1 N2 N 0.5634(17) 0.1349(10) 0.4907(11) 0.122(6) Uani 0.59(2) 1 d PDU A 1 C14 C 0.738(2) 0.131(2) 0.497(3) 0.132(10) Uani 0.59(2) 1 d PDU A 1 C15 C 0.481(4) 0.181(2) 0.564(2) 0.123(11) Uani 0.59(2) 1 d PDU A 1 O7' O 0.377(3) 0.063(3) 0.402(4) 0.136(12) Uani 0.41(2) 1 d PDU A 2 C12' C 0.479(3) 0.1130(19) 0.458(2) 0.127(9) Uani 0.41(2) 1 d PDU A 2 C13' C 0.443(5) 0.180(3) 0.535(3) 0.101(11) Uani 0.41(2) 1 d PDU A 2 N2' N 0.614(3) 0.0975(14) 0.4425(16) 0.131(8) Uani 0.41(2) 1 d PDU A 2 C14' C 0.725(3) 0.155(4) 0.526(5) 0.128(13) Uani 0.41(2) 1 d PDU A 2 C15' C 0.639(4) 0.0303(19) 0.366(2) 0.102(9) Uani 0.41(2) 1 d PDU A 2 C1 C 0.2061(4) 0.1276(3) 0.8420(3) 0.0336(10) Uani 1 1 d . . . C2 C 0.0643(4) 0.1222(3) 0.8619(3) 0.0351(11) Uani 1 1 d . . . H2 H 0.0420 0.0821 0.9094 0.042 Uiso 1 1 calc R . . C3 C -0.0440(4) 0.1760(3) 0.8118(3) 0.0352(11) Uani 1 1 d . . . C4 C -0.0113(5) 0.2343(3) 0.7398(4) 0.0406(11) Uani 1 1 d . . . H4 H -0.0845 0.2691 0.7042 0.049 Uiso 1 1 calc R . . C5 C 0.1302(5) 0.2415(3) 0.7199(4) 0.0424(12) Uani 1 1 d . . . C6 C 0.2375(5) 0.1882(3) 0.7720(4) 0.0409(12) Uani 1 1 d . . . H6 H 0.3324 0.1932 0.7597 0.049 Uiso 1 1 calc R . . C7 C 0.3209(5) 0.0680(3) 0.8970(3) 0.0349(11) Uani 1 1 d . . . C8 C -0.1966(5) 0.1695(3) 0.8377(4) 0.0395(11) Uani 1 1 d . . . C9 C 0.1673(6) 0.3062(3) 0.6431(4) 0.0521(13) Uani 1 1 d . . . C10 C 0.0290(10) 0.0708(7) 0.3241(8) 0.200(6) Uani 1 1 d . . . H10A H -0.0600 0.0470 0.2851 0.300 Uiso 1 1 calc R . . H10B H 0.0092 0.1003 0.3859 0.300 Uiso 1 1 calc R . . H10C H 0.0985 0.0274 0.3475 0.300 Uiso 1 1 calc R . . C11 C 0.1282(8) 0.0934(5) 0.1580(6) 0.105(3) Uani 1 1 d . . . H11A H 0.1935 0.0472 0.1757 0.158 Uiso 1 1 calc R . . H11B H 0.1762 0.1365 0.1252 0.158 Uiso 1 1 calc R . . H11C H 0.0425 0.0757 0.1084 0.158 Uiso 1 1 calc R . . N1 N 0.0860(7) 0.1255(4) 0.2570(5) 0.107(2) Uani 1 1 d . . . H1A H 0.1654 0.1496 0.2969 0.128 Uiso 1 1 calc R . . H1B H 0.0195 0.1658 0.2374 0.128 Uiso 1 1 calc R . . O1 O 0.4463(3) 0.0743(2) 0.8750(2) 0.0428(8) Uani 1 1 d . . . O2 O 0.2835(3) 0.0171(2) 0.9609(3) 0.0460(8) Uani 1 1 d . . . O3 O -0.2141(3) 0.1088(2) 0.8980(3) 0.0473(9) Uani 1 1 d . . . O4 O -0.2902(4) 0.2200(2) 0.8016(3) 0.0705(12) Uani 1 1 d . . . O5 O 0.0633(4) 0.3360(2) 0.5755(3) 0.0567(10) Uani 1 1 d . . . O6 O 0.2970(4) 0.3267(3) 0.6484(3) 0.0833(14) Uani 1 1 d . . . Zn1 Zn 0.63271(5) 0.08742(3) 0.97674(4) 0.03157(18) 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 O7 0.115(11) 0.144(19) 0.141(14) -0.002(14) -0.034(9) 0.008(10) C12 0.191(18) 0.091(12) 0.061(10) 0.013(9) 0.013(12) -0.018(14) C13 0.21(2) 0.094(12) 0.076(13) -0.014(10) 0.021(13) 0.059(13) N2 0.165(15) 0.103(11) 0.092(11) 0.010(8) 0.009(10) -0.013(10) C14 0.103(15) 0.15(2) 0.13(2) -0.031(15) -0.007(14) -0.036(14) C15 0.145(17) 0.139(17) 0.08(2) -0.043(15) 0.008(14) 0.023(13) O7' 0.17(3) 0.13(2) 0.094(15) -0.002(17) -0.008(18) -0.014(19) C12' 0.20(2) 0.109(18) 0.071(17) 0.014(14) 0.013(17) -0.007(17) C13' 0.17(3) 0.106(19) 0.026(12) -0.017(11) 0.018(17) 0.030(19) N2' 0.193(18) 0.125(16) 0.080(14) 0.010(12) 0.038(14) -0.005(15) C14' 0.085(17) 0.17(3) 0.13(3) -0.057(19) 0.017(15) -0.004(16) C15' 0.15(2) 0.12(2) 0.044(13) -0.010(13) 0.029(14) 0.020(17) C1 0.028(2) 0.039(3) 0.035(2) 0.003(2) 0.0086(19) 0.0026(19) C2 0.030(2) 0.037(3) 0.040(3) 0.006(2) 0.010(2) -0.003(2) C3 0.027(2) 0.038(3) 0.043(3) 0.004(2) 0.011(2) -0.0005(19) C4 0.031(3) 0.043(3) 0.049(3) 0.010(2) 0.009(2) 0.005(2) C5 0.033(3) 0.042(3) 0.054(3) 0.016(2) 0.013(2) -0.002(2) C6 0.028(2) 0.048(3) 0.050(3) 0.009(2) 0.016(2) -0.003(2) C7 0.028(2) 0.041(3) 0.035(2) -0.005(2) 0.006(2) -0.0004(19) C8 0.031(3) 0.044(3) 0.044(3) 0.004(2) 0.009(2) 0.003(2) C9 0.047(3) 0.051(3) 0.060(3) 0.012(3) 0.015(3) 0.000(3) C10 0.098(7) 0.307(17) 0.202(11) 0.130(11) 0.044(7) -0.010(8) C11 0.102(6) 0.103(6) 0.109(6) -0.050(5) 0.018(5) 0.004(4) N1 0.123(5) 0.095(5) 0.107(5) -0.031(4) 0.031(4) -0.027(4) O1 0.0266(17) 0.061(2) 0.0405(17) 0.0012(16) 0.0051(13) 0.0027(15) O2 0.0340(18) 0.045(2) 0.061(2) 0.0227(17) 0.0158(16) 0.0101(15) O3 0.0362(19) 0.047(2) 0.065(2) 0.0141(17) 0.0241(16) 0.0021(15) O4 0.037(2) 0.067(3) 0.111(3) 0.038(2) 0.022(2) 0.0161(19) O5 0.045(2) 0.066(3) 0.060(2) 0.028(2) 0.0124(18) 0.0024(18) O6 0.042(2) 0.093(3) 0.117(3) 0.056(3) 0.022(2) -0.007(2) Zn1 0.0228(3) 0.0343(3) 0.0393(3) -0.0001(3) 0.01030(19) 0.0021(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 O7 C12 1.35(2) . ? C12 N2 1.335(17) . ? C12 C13 1.525(14) . ? N2 C15 1.505(14) . ? N2 C14 1.62(2) . ? O7' C12' 1.34(3) . ? C12' N2' 1.342(19) . ? C12' C13' 1.524(15) . ? N2' C15' 1.500(14) . ? N2' C14' 1.62(2) . ? C1 C6 1.384(6) . ? C1 C2 1.394(5) . ? C1 C7 1.506(6) . ? C2 C3 1.388(6) . ? C2 H2 0.9300 . ? C3 C4 1.379(6) . ? C3 C8 1.522(6) . ? C4 C5 1.394(6) . ? C4 H4 0.9300 . ? C5 C6 1.385(6) . ? C5 C9 1.506(7) . ? C6 H6 0.9300 . ? C7 O2 1.244(5) . ? C7 O1 1.256(5) . ? C8 O4 1.216(5) . ? C8 O3 1.269(5) . ? C9 O6 1.243(6) . ? C9 O5 1.258(6) . ? C10 N1 1.394(9) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N1 1.472(8) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? O1 Zn1 1.965(3) . ? O2 Zn1 1.957(3) 3_657 ? O3 Zn1 1.918(3) 1_455 ? O5 Zn1 1.949(3) 4_565 ? Zn1 O3 1.918(3) 1_655 ? Zn1 O5 1.949(3) 4_666 ? Zn1 O2 1.957(3) 3_657 ? 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 N2 C12 O7 114(2) . . ? N2 C12 C13 125.6(17) . . ? O7 C12 C13 120(2) . . ? C12 N2 C15 122.0(16) . . ? C12 N2 C14 109.5(15) . . ? C15 N2 C14 128.5(17) . . ? N2' C12' O7' 114(3) . . ? N2' C12' C13' 123(2) . . ? O7' C12' C13' 123(3) . . ? C12' N2' C15' 119.6(18) . . ? C12' N2' C14' 107.3(18) . . ? C15' N2' C14' 133(2) . . ? C6 C1 C2 118.8(4) . . ? C6 C1 C7 121.7(4) . . ? C2 C1 C7 119.5(4) . . ? C3 C2 C1 120.7(4) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 119.5(4) . . ? C4 C3 C8 121.4(4) . . ? C2 C3 C8 119.1(4) . . ? C3 C4 C5 120.7(4) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 119.0(4) . . ? C6 C5 C9 120.0(4) . . ? C4 C5 C9 120.9(4) . . ? C1 C6 C5 121.2(4) . . ? C1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? O2 C7 O1 125.7(4) . . ? O2 C7 C1 117.2(4) . . ? O1 C7 C1 117.2(4) . . ? O4 C8 O3 125.1(4) . . ? O4 C8 C3 120.5(4) . . ? O3 C8 C3 114.5(4) . . ? O6 C9 O5 123.4(5) . . ? O6 C9 C5 119.3(5) . . ? O5 C9 C5 117.3(4) . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 N1 C11 119.2(8) . . ? C10 N1 H1A 107.5 . . ? C11 N1 H1A 107.5 . . ? C10 N1 H1B 107.5 . . ? C11 N1 H1B 107.5 . . ? H1A N1 H1B 107.0 . . ? C7 O1 Zn1 127.6(3) . . ? C7 O2 Zn1 133.4(3) . 3_657 ? C8 O3 Zn1 129.9(3) . 1_455 ? C9 O5 Zn1 111.6(3) . 4_565 ? O3 Zn1 O5 125.96(15) 1_655 4_666 ? O3 Zn1 O2 94.75(13) 1_655 3_657 ? O5 Zn1 O2 116.33(15) 4_666 3_657 ? O3 Zn1 O1 109.52(14) 1_655 . ? O5 Zn1 O1 97.20(14) 4_666 . ? O2 Zn1 O1 113.94(14) 3_657 . ? 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 O7 C12 N2 C15 8(4) . . . . ? C13 C12 N2 C15 179(3) . . . . ? O7 C12 N2 C14 -175(3) . . . . ? C13 C12 N2 C14 -4(3) . . . . ? O7' C12' N2' C15' 1(4) . . . . ? C13' C12' N2' C15' 180(3) . . . . ? O7' C12' N2' C14' -173(4) . . . . ? C13' C12' N2' C14' 5(5) . . . . ? C6 C1 C2 C3 0.6(7) . . . . ? C7 C1 C2 C3 -179.6(4) . . . . ? C1 C2 C3 C4 1.3(7) . . . . ? C1 C2 C3 C8 -178.5(4) . . . . ? C2 C3 C4 C5 -2.3(7) . . . . ? C8 C3 C4 C5 177.6(4) . . . . ? C3 C4 C5 C6 1.3(7) . . . . ? C3 C4 C5 C9 -178.8(4) . . . . ? C2 C1 C6 C5 -1.7(7) . . . . ? C7 C1 C6 C5 178.5(4) . . . . ? C4 C5 C6 C1 0.8(7) . . . . ? C9 C5 C6 C1 -179.2(4) . . . . ? C6 C1 C7 O2 178.1(4) . . . . ? C2 C1 C7 O2 -1.8(6) . . . . ? C6 C1 C7 O1 -1.4(6) . . . . ? C2 C1 C7 O1 178.8(4) . . . . ? C4 C3 C8 O4 -5.7(7) . . . . ? C2 C3 C8 O4 174.2(5) . . . . ? C4 C3 C8 O3 174.3(4) . . . . ? C2 C3 C8 O3 -5.9(6) . . . . ? C6 C5 C9 O6 -19.4(8) . . . . ? C4 C5 C9 O6 160.6(5) . . . . ? C6 C5 C9 O5 159.8(5) . . . . ? C4 C5 C9 O5 -20.1(7) . . . . ? O2 C7 O1 Zn1 -53.2(6) . . . . ? C1 C7 O1 Zn1 126.2(4) . . . . ? O1 C7 O2 Zn1 -18.6(7) . . . 3_657 ? C1 C7 O2 Zn1 162.0(3) . . . 3_657 ? O4 C8 O3 Zn1 -14.7(8) . . . 1_455 ? C3 C8 O3 Zn1 165.3(3) . . . 1_455 ? O6 C9 O5 Zn1 3.2(7) . . . 4_565 ? C5 C9 O5 Zn1 -176.1(3) . . . 4_565 ? C7 O1 Zn1 O3 -172.4(3) . . . 1_655 ? C7 O1 Zn1 O5 -40.1(4) . . . 4_666 ? C7 O1 Zn1 O2 82.9(4) . . . 3_657 ? 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 N1 H1B O6 0.90 2.17 2.885(8) 136.4 4_565 N1 H1A O4 0.90 2.14 2.757(7) 125.0 4_665 N1 H1A O7 0.90 2.12 2.77(2) 128.2 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.461 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.082 data_5 _database_code_depnum_ccdc_archive 'CCDC 838773' #TrackingRef '- MOF1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Zn3(C9H3O6)3 3(C2H8N) 4(C4H9NO)' _chemical_formula_sum 'C49 H69 N7 O22 Zn3' _chemical_formula_weight 1304.34 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 R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'y+2/3, x+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'y+1/3, x+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-y+2/3, -x+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-y+1/3, -x+2/3, z+1/6' _cell_length_a 43.648(5) _cell_length_b 43.648(5) _cell_length_c 17.371(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 120.000 _cell_volume 28661(9) _cell_formula_units_Z 18 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4489 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7290.0 _exptl_absorpt_coefficient_mu 1.668 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4402 _exptl_absorpt_correction_T_max 0.5623 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 47448 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 0.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5621 _reflns_number_gt 3927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 'SHELXTL and local programs' _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^)+(0.1300P)^2^+142.8672P] 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 5621 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.2218 _refine_ls_wR_factor_gt 0.1923 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.115 _refine_ls_shift/su_mean 0.156 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 0.844073(16) 0.018014(16) 1.15992(3) 0.0328(2) Uani 1 1 d . . . Zn2 Zn 0.74257(2) 0.0000 0.7500 0.0431(3) Uani 1 2 d S . . C1 C 0.87989(15) 0.08137(18) 0.7915(3) 0.0487(16) Uani 1 1 d . . . H1 H 0.8816 0.0879 0.7400 0.058 Uiso 1 1 calc R . . C2 C 0.91042(15) 0.09346(17) 0.8355(3) 0.0435(14) Uani 1 1 d . . . C3 C 0.68836(18) 0.07357(17) 0.6336(4) 0.0510(16) Uani 1 1 d . . . H3 H 0.7024 0.0913 0.6682 0.061 Uiso 1 1 calc R . . C4 C 0.81415(18) 0.0467(2) 0.7762(4) 0.063(2) Uani 1 1 d . . . C5 C 0.87470(18) 0.06004(19) 0.9433(3) 0.0531(17) Uani 1 1 d . . . C6 C 0.68935(19) 0.04206(18) 0.6326(4) 0.0560(18) Uani 1 1 d . . . C7 C 0.90779(17) 0.08239(19) 0.9115(3) 0.0523(17) Uani 1 1 d . . . H7 H 0.9281 0.0899 0.9410 0.063 Uiso 1 1 calc R . . C8 C 0.84499(17) 0.04968(19) 0.9000(4) 0.0549(17) Uani 1 1 d . . . H8 H 0.8229 0.0355 0.9223 0.066 Uiso 1 1 calc R . . C9 C 0.84695(16) 0.05977(18) 0.8238(4) 0.0499(16) Uani 1 1 d . . . C10 C 0.6667 0.11256(19) 0.5833 0.047(2) Uani 1 2 d S . . C11 C 0.6667 0.07850(19) 0.5833 0.046(2) Uani 1 2 d S . . C12 C 0.94551(16) 0.11817(16) 0.8013(3) 0.0424(14) Uani 1 1 d . . . C13 C 0.7139(2) 0.0376(2) 0.6854(5) 0.069(2) Uani 1 1 d . . . C14 C 0.8723(2) 0.0473(2) 1.0251(4) 0.064(2) Uani 1 1 d . . . C15 C 0.6667 0.0148(2) 0.5833 0.056(3) Uani 1 2 d S . . H15 H 0.6667 -0.0065 0.5833 0.067 Uiso 1 2 calc SR . . O1 O 0.7260(2) 0.0571(2) 0.7412(5) 0.134(3) Uani 1 1 d . . . O2 O 0.72164(14) 0.01455(14) 0.6676(3) 0.0662(14) Uani 1 1 d . . . O3 O 0.65577(16) 0.12007(13) 0.5245(3) 0.0692(15) Uani 1 1 d . . . O4 O 0.78494(11) 0.02976(14) 0.8108(3) 0.0629(13) Uani 1 1 d . . . O5 O 0.81673(15) 0.0523(2) 0.7065(4) 0.124(3) Uani 1 1 d . . . O6 O 0.84323(13) 0.03321(14) 1.0559(3) 0.0653(14) Uani 1 1 d . . . O7 O 0.8978(2) 0.0502(3) 1.0588(4) 0.140(4) Uani 1 1 d . . . O8 O 0.97175(11) 0.13190(13) 0.8455(3) 0.0593(13) Uani 1 1 d . . . O9 O 0.94663(11) 0.12357(13) 0.7306(2) 0.0616(14) 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 0.0368(4) 0.0330(4) 0.0229(4) 0.0022(2) -0.0001(2) 0.0132(3) Zn2 0.0359(4) 0.0557(6) 0.0445(6) 0.0048(5) 0.0024(2) 0.0278(3) C1 0.039(3) 0.065(4) 0.031(3) 0.018(3) 0.003(2) 0.017(3) C2 0.035(3) 0.054(4) 0.029(3) 0.009(3) 0.004(2) 0.013(3) C3 0.060(4) 0.041(3) 0.056(4) -0.015(3) -0.027(3) 0.028(3) C4 0.039(4) 0.075(5) 0.058(4) 0.024(4) -0.005(3) 0.016(3) C5 0.049(4) 0.067(4) 0.032(3) 0.017(3) 0.004(3) 0.020(3) C6 0.063(4) 0.052(4) 0.064(4) -0.011(3) -0.023(3) 0.037(4) C7 0.039(3) 0.073(5) 0.028(3) 0.008(3) -0.001(3) 0.016(3) C8 0.040(4) 0.070(4) 0.041(3) 0.019(3) 0.013(3) 0.018(3) C9 0.031(3) 0.065(4) 0.041(3) 0.016(3) 0.002(3) 0.015(3) C10 0.056(5) 0.042(3) 0.047(5) -0.005(2) -0.011(4) 0.028(3) C11 0.053(5) 0.040(3) 0.049(5) -0.008(2) -0.015(4) 0.026(3) C12 0.038(3) 0.044(3) 0.035(3) 0.002(3) 0.000(3) 0.014(3) C13 0.078(5) 0.056(5) 0.081(5) -0.015(4) -0.039(4) 0.039(4) C14 0.064(5) 0.084(5) 0.035(3) 0.016(4) 0.002(3) 0.029(4) C15 0.057(6) 0.041(3) 0.076(7) -0.012(3) -0.023(5) 0.028(3) O1 0.192(8) 0.118(6) 0.143(6) -0.070(5) -0.125(6) 0.116(6) O2 0.080(4) 0.076(4) 0.066(3) -0.002(3) -0.019(3) 0.057(3) O3 0.113(4) 0.060(3) 0.056(3) -0.012(2) -0.035(3) 0.058(3) O4 0.033(2) 0.083(4) 0.063(3) 0.004(3) -0.003(2) 0.021(2) O5 0.052(3) 0.184(7) 0.066(4) 0.056(4) -0.014(3) 0.006(4) O6 0.066(3) 0.077(3) 0.035(2) 0.022(2) 0.014(2) 0.022(3) O7 0.098(5) 0.248(10) 0.061(4) 0.063(5) -0.003(4) 0.076(6) O8 0.036(2) 0.068(3) 0.048(3) 0.014(2) -0.005(2) 0.007(2) O9 0.042(3) 0.077(3) 0.032(2) 0.009(2) 0.0065(19) 0.004(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 O9 1.924(4) 24_666 y Zn1 O6 1.932(4) . y Zn1 O8 1.936(4) 21_547 y Zn1 O3 1.967(5) 15_655 y Zn2 O4 1.954(5) 4_556 y Zn2 O4 1.954(5) . y Zn2 O2 1.967(4) . y Zn2 O2 1.967(4) 4_556 y C1 C9 1.383(8) . ? C1 C2 1.391(8) . ? C2 C7 1.392(8) . ? C2 C12 1.487(8) . ? C3 C11 1.381(7) . ? C3 C6 1.397(9) . ? C4 O5 1.229(9) . ? C4 O4 1.261(8) . ? C4 C9 1.497(9) . ? C5 C8 1.365(9) . ? C5 C7 1.390(9) . ? C5 C14 1.511(8) . ? C6 C15 1.398(8) . ? C6 C13 1.497(9) . ? C8 C9 1.385(8) . ? C10 O3 1.238(6) 17_655 ? C10 O3 1.238(6) . ? C10 C11 1.487(12) . ? C11 C3 1.381(7) 17_655 ? C12 O9 1.246(7) . ? C12 O8 1.255(7) . ? C13 O1 1.224(9) . ? C13 O2 1.247(9) . ? C14 O7 1.205(9) . ? C14 O6 1.223(8) . ? C15 C6 1.398(8) 17_655 ? O3 Zn1 1.968(4) 8_544 ? O8 Zn1 1.936(4) 20_667 ? O9 Zn1 1.925(4) 24_665 ? 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 O9 Zn1 O6 117.0(2) 24_666 . y O9 Zn1 O8 121.1(2) 24_666 21_547 y O6 Zn1 O8 107.8(2) . 21_547 y O9 Zn1 O3 103.6(2) 24_666 15_655 y O6 Zn1 O3 96.8(2) . 15_655 ? O8 Zn1 O3 107.2(2) 21_547 15_655 y O4 Zn2 O4 104.2(3) 4_556 . y O4 Zn2 O2 98.7(2) 4_556 . y O4 Zn2 O2 128.1(2) . . y O4 Zn2 O2 128.1(2) 4_556 4_556 y O4 Zn2 O2 98.7(2) . 4_556 y O2 Zn2 O2 102.5(3) . 4_556 y C9 C1 C2 120.6(5) . . ? C7 C2 C1 119.5(5) . . ? C7 C2 C12 120.5(5) . . ? C1 C2 C12 120.0(5) . . ? C11 C3 C6 120.5(6) . . ? O5 C4 O4 123.5(6) . . ? O5 C4 C9 119.5(6) . . ? O4 C4 C9 117.0(6) . . ? C8 C5 C7 119.7(5) . . ? C8 C5 C14 121.1(6) . . ? C7 C5 C14 119.2(6) . . ? C15 C6 C3 119.2(6) . . ? C15 C6 C13 120.8(6) . . ? C3 C6 C13 119.9(6) . . ? C2 C7 C5 119.8(6) . . ? C5 C8 C9 121.6(6) . . ? C8 C9 C1 118.8(6) . . ? C8 C9 C4 120.8(6) . . ? C1 C9 C4 120.4(5) . . ? O3 C10 O3 125.7(8) 17_655 . ? O3 C10 C11 117.2(4) 17_655 . ? O3 C10 C11 117.2(4) . . ? C3 C11 C3 120.2(8) . 17_655 ? C3 C11 C10 119.9(4) . . ? C3 C11 C10 119.9(4) 17_655 . ? O9 C12 O8 124.9(6) . . ? O9 C12 C2 117.4(5) . . ? O8 C12 C2 117.7(5) . . ? O1 C13 O2 124.3(7) . . ? O1 C13 C6 118.7(7) . . ? O2 C13 C6 116.9(6) . . ? O7 C14 O6 120.8(7) . . ? O7 C14 C5 121.8(7) . . ? O6 C14 C5 117.3(7) . . ? C6 C15 C6 120.3(8) 17_655 . ? C13 O2 Zn2 115.8(5) . . ? C10 O3 Zn1 135.1(5) . 8_544 ? C4 O4 Zn2 118.4(5) . . ? C14 O6 Zn1 112.8(5) . . ? C12 O8 Zn1 133.9(4) . 20_667 ? C12 O9 Zn1 135.1(4) . 24_665 ? 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 _platon_squeeze_void_content 1 -0.018 -0.010 -0.011 18916 4948 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.798 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.181 data_6 _database_code_depnum_ccdc_archive 'CCDC 838774' #TrackingRef '- MOF1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Zn9(C9H6O6)6(OH)2 .2(C2H8N). 15(C4H9NO)' _chemical_formula_sum 'C118 H189 N17 O53 Zn9' _chemical_formula_weight 3282.19 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 cubic _symmetry_space_group_name_H-M 'I 2 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' 'z, x, y' 'y, z, x' '-z, -x, y' '-y, z, -x' 'z, -x, -y' '-y, -z, x' '-z, x, -y' 'y, -z, -x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'y+1/2, z+1/2, x+1/2' '-z+1/2, -x+1/2, y+1/2' '-y+1/2, z+1/2, -x+1/2' 'z+1/2, -x+1/2, -y+1/2' '-y+1/2, -z+1/2, x+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, -z+1/2, -x+1/2' _cell_length_a 23.461(5) _cell_length_b 23.461(5) _cell_length_c 23.461(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 12913(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5586 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6840 _exptl_absorpt_coefficient_mu 1.743 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8077 _exptl_absorpt_correction_T_max 0.8116 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 36456 _diffrn_reflns_av_R_equivalents 0.0791 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 26.24 _reflns_number_total 4356 _reflns_number_gt 3404 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 'SHELXTL and local programs' _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^)+(0.0414P)^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 0.000(16) _refine_ls_number_reflns 4356 _refine_ls_number_parameters 165 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.015 _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 0.5000 0.0000 0.93658(2) 0.03060(14) Uani 1 2 d S . . Zn2 Zn 0.75923(2) 0.29464(2) 0.81543(2) 0.04639(14) Uani 1 1 d . . . C1 C 0.64490(17) 0.13927(16) 0.94329(18) 0.0414(10) Uani 1 1 d . . . H1 H 0.6343 0.1203 0.9101 0.14(3) Uiso 1 1 calc R . . C2 C 0.68529(17) 0.18277(17) 0.94018(16) 0.0410(9) Uani 1 1 d . . . C3 C 0.70113(17) 0.21058(17) 0.98867(16) 0.0469(10) Uani 1 1 d . . . H3 H 0.7284 0.2393 0.9867 0.054(12) Uiso 1 1 calc R . . C4 C 0.67701(19) 0.19664(17) 1.04135(16) 0.0477(11) Uani 1 1 d . . . C5 C 0.63602(19) 0.15274(18) 1.04352(18) 0.0480(11) Uani 1 1 d . . . H5 H 0.6193 0.1431 1.0782 0.025(9) Uiso 1 1 calc R . . C6 C 0.62030(16) 0.12368(15) 0.99433(18) 0.0407(9) Uani 1 1 d . . . C7 C 0.70744(16) 0.20105(17) 0.88232(17) 0.0389(9) Uani 1 1 d . . . C8 C 0.57696(16) 0.07796(16) 0.9981(2) 0.0456(9) Uani 1 1 d . . . C9 C 0.7296(2) 0.40581(19) 0.8070(2) 0.0586(13) Uani 1 1 d . . . N1? N 0.6781(2) 0.3219(2) 0.6781(2) 0.118(3) Uani 1 3 d S . . O1 O 0.73723(13) 0.24473(13) 0.88089(12) 0.0573(8) Uani 1 1 d . . . O2 O 0.84057(12) 0.30450(14) 0.83059(12) 0.0585(8) Uani 1 1 d . . . O3 O 0.55669(13) 0.06610(13) 1.04546(13) 0.0543(8) Uani 1 1 d . . . O4 O 0.56379(13) 0.05514(13) 0.95116(13) 0.0584(8) Uani 1 1 d . . . O5 O 0.71494(13) 0.36085(13) 0.83253(14) 0.0608(9) Uani 1 1 d . . . O6 O 0.76601(19) 0.40753(15) 0.77105(19) 0.1080(15) Uani 1 1 d . . . O7 O 0.74454(11) 0.25546(11) 0.74454(11) 0.0403(11) Uani 1 3 d S . . O8 O 0.5000 0.0000 0.85335(17) 0.0963(18) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0387(3) 0.0282(3) 0.0249(3) 0.000 0.000 -0.0031(3) Zn2 0.0429(3) 0.0336(3) 0.0627(4) -0.0030(2) 0.0116(2) 0.0009(2) C1 0.053(3) 0.032(2) 0.039(2) -0.0108(19) 0.004(2) -0.0109(19) C2 0.046(2) 0.047(2) 0.030(2) -0.0068(19) 0.0098(18) -0.009(2) C3 0.047(2) 0.052(2) 0.042(3) -0.005(2) 0.0043(19) -0.015(2) C4 0.065(3) 0.042(2) 0.036(2) -0.0070(19) -0.008(2) -0.012(2) C5 0.063(3) 0.047(3) 0.033(2) 0.008(2) 0.006(2) -0.002(2) C6 0.057(2) 0.033(2) 0.032(2) -0.0007(19) -0.001(2) -0.0101(18) C7 0.033(2) 0.038(2) 0.045(2) 0.0005(19) 0.0095(19) 0.0031(19) C8 0.043(2) 0.042(2) 0.052(2) -0.014(2) 0.008(2) -0.0079(17) C9 0.061(3) 0.047(3) 0.068(3) -0.008(3) 0.016(3) 0.011(2) N1? 0.118(3) 0.118(3) 0.118(3) 0.025(3) -0.025(3) 0.025(3) O1 0.068(2) 0.0529(19) 0.0505(18) 0.0048(15) -0.0003(16) -0.0272(16) O2 0.0382(17) 0.082(2) 0.0556(19) -0.0201(17) 0.0040(14) -0.0095(16) O3 0.064(2) 0.0470(18) 0.0523(19) -0.0030(15) 0.0141(16) -0.0226(16) O4 0.060(2) 0.059(2) 0.055(2) -0.0124(16) 0.0036(16) -0.0217(16) O5 0.059(2) 0.0462(19) 0.077(2) -0.0082(16) 0.0227(18) 0.0141(16) O6 0.125(3) 0.064(2) 0.134(4) 0.007(2) 0.088(3) 0.023(2) O7 0.0403(11) 0.0403(11) 0.0403(11) 0.0024(12) -0.0024(12) 0.0024(12) O8 0.186(6) 0.070(3) 0.033(2) 0.000 0.000 -0.041(4) _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 O8 1.953(4) . ? Zn1 O4 2.008(3) 2_655 ? Zn1 O4 2.008(3) . ? Zn1 O3 2.086(3) 4_657 ? Zn1 O3 2.086(3) 3_557 ? Zn1 Zn1 2.9759(12) 3_557 ? Zn2 O5 1.912(3) . ? Zn2 O7 1.9312(16) . ? Zn2 O2 1.955(3) . ? Zn2 O1 1.999(3) . ? C1 C6 1.379(6) . ? C1 C2 1.394(5) . ? C1 H1 0.9300 . ? C2 C3 1.363(5) . ? C2 C7 1.516(5) . ? C3 C4 1.398(5) . ? C3 H3 0.9300 . ? C4 C5 1.410(6) . ? C4 C9 1.509(5) 23_646 ? C5 C6 1.390(5) . ? C5 H5 0.9300 . ? C6 C8 1.481(5) . ? C7 O1 1.241(5) . ? C7 O2 1.261(5) 10_665 ? C8 O3 1.240(5) . ? C8 O4 1.263(5) . ? C9 O6 1.201(5) . ? C9 O5 1.261(5) . ? C9 C4 1.509(5) 24_566 ? O2 C7 1.261(5) 9_566 ? O3 Zn1 2.086(3) 3_557 ? O7 Zn2 1.9312(16) 9_566 ? O7 Zn2 1.9312(16) 10_665 ? 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 O8 Zn1 O4 99.81(9) . 2_655 ? O8 Zn1 O4 99.81(9) . . ? O4 Zn1 O4 160.38(18) 2_655 . ? O8 Zn1 O3 101.66(8) . 4_657 ? O4 Zn1 O3 88.25(12) 2_655 4_657 ? O4 Zn1 O3 87.81(12) . 4_657 ? O8 Zn1 O3 101.66(8) . 3_557 ? O4 Zn1 O3 87.81(12) 2_655 3_557 ? O4 Zn1 O3 88.25(12) . 3_557 ? O3 Zn1 O3 156.69(17) 4_657 3_557 ? O8 Zn1 Zn1 180.0 . 3_557 ? O4 Zn1 Zn1 80.19(9) 2_655 3_557 ? O4 Zn1 Zn1 80.19(9) . 3_557 ? O3 Zn1 Zn1 78.34(8) 4_657 3_557 ? O3 Zn1 Zn1 78.34(8) 3_557 3_557 ? O5 Zn2 O7 118.07(16) . . ? O5 Zn2 O2 113.34(14) . . ? O7 Zn2 O2 112.78(11) . . ? O5 Zn2 O1 100.05(14) . . ? O7 Zn2 O1 109.68(11) . . ? O2 Zn2 O1 100.46(13) . . ? C6 C1 C2 121.6(4) . . ? C6 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 119.5(4) . . ? C3 C2 C7 121.2(3) . . ? C1 C2 C7 119.1(3) . . ? C2 C3 C4 121.0(4) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C3 C4 C5 118.6(4) . . ? C3 C4 C9 120.4(4) . 23_646 ? C5 C4 C9 121.0(4) . 23_646 ? C6 C5 C4 120.6(4) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C1 C6 C5 118.7(3) . . ? C1 C6 C8 122.1(4) . . ? C5 C6 C8 119.2(4) . . ? O1 C7 O2 126.2(4) . 10_665 ? O1 C7 C2 116.8(4) . . ? O2 C7 C2 116.9(4) 10_665 . ? O3 C8 O4 126.3(3) . . ? O3 C8 C6 118.6(4) . . ? O4 C8 C6 115.0(4) . . ? O6 C9 O5 123.8(4) . . ? O6 C9 C4 120.8(5) . 24_566 ? O5 C9 C4 115.4(4) . 24_566 ? C7 O1 Zn2 130.5(3) . . ? C7 O2 Zn2 128.7(3) 9_566 . ? C8 O3 Zn1 126.3(3) . 3_557 ? C8 O4 Zn1 127.2(3) . . ? C9 O5 Zn2 115.6(3) . . ? Zn2 O7 Zn2 109.95(12) . 9_566 ? Zn2 O7 Zn2 109.95(12) . 10_665 ? Zn2 O7 Zn2 109.95(12) 9_566 10_665 ? 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 C6 C1 C2 C3 0.2(6) . . . . ? C6 C1 C2 C7 -175.3(4) . . . . ? C1 C2 C3 C4 -0.8(6) . . . . ? C7 C2 C3 C4 174.7(4) . . . . ? C2 C3 C4 C5 0.4(6) . . . . ? C2 C3 C4 C9 -177.2(4) . . . 23_646 ? C3 C4 C5 C6 0.5(6) . . . . ? C9 C4 C5 C6 178.1(4) 23_646 . . . ? C2 C1 C6 C5 0.7(6) . . . . ? C2 C1 C6 C8 179.4(4) . . . . ? C4 C5 C6 C1 -1.0(6) . . . . ? C4 C5 C6 C8 -179.8(4) . . . . ? C3 C2 C7 O1 -5.0(6) . . . . ? C1 C2 C7 O1 170.5(4) . . . . ? C3 C2 C7 O2 172.7(4) . . . 10_665 ? C1 C2 C7 O2 -11.9(6) . . . 10_665 ? C1 C6 C8 O3 179.9(4) . . . . ? C5 C6 C8 O3 -1.4(6) . . . . ? C1 C6 C8 O4 -1.0(6) . . . . ? C5 C6 C8 O4 177.7(4) . . . . ? O2 C7 O1 Zn2 19.4(6) 10_665 . . . ? C2 C7 O1 Zn2 -163.2(3) . . . . ? O5 Zn2 O1 C7 109.2(4) . . . . ? O7 Zn2 O1 C7 -15.6(4) . . . . ? O2 Zn2 O1 C7 -134.6(4) . . . . ? O5 Zn2 O2 C7 -131.9(3) . . . 9_566 ? O7 Zn2 O2 C7 5.6(4) . . . 9_566 ? O1 Zn2 O2 C7 122.2(4) . . . 9_566 ? O4 C8 O3 Zn1 5.9(6) . . . 3_557 ? C6 C8 O3 Zn1 -175.1(3) . . . 3_557 ? O3 C8 O4 Zn1 8.1(6) . . . . ? C6 C8 O4 Zn1 -170.9(3) . . . . ? O8 Zn1 O4 C8 168.4(3) . . . . ? O4 Zn1 O4 C8 -11.6(3) 2_655 . . . ? O3 Zn1 O4 C8 66.9(4) 4_657 . . . ? O3 Zn1 O4 C8 -90.1(4) 3_557 . . . ? Zn1 Zn1 O4 C8 -11.6(3) 3_557 . . . ? O6 C9 O5 Zn2 5.2(7) . . . . ? C4 C9 O5 Zn2 -176.8(3) 24_566 . . . ? O7 Zn2 O5 C9 -78.0(3) . . . . ? O2 Zn2 O5 C9 57.1(4) . . . . ? O1 Zn2 O5 C9 163.2(3) . . . . ? O5 Zn2 O7 Zn2 131.76(18) . . . 9_566 ? O2 Zn2 O7 Zn2 -3.6(2) . . . 9_566 ? O1 Zn2 O7 Zn2 -114.61(16) . . . 9_566 ? O5 Zn2 O7 Zn2 -107.1(2) . . . 10_665 ? O2 Zn2 O7 Zn2 117.63(15) . . . 10_665 ? O1 Zn2 O7 Zn2 6.6(2) . . . 10_665 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.24 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.635 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.053 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 -0.021 -0.005 -0.001 7720 2587 ' ' _platon_squeeze_details ; ; data_7 _database_code_depnum_ccdc_archive 'CCDC 838775' #TrackingRef '- MOF1-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Zn9(C9H3O6)5(OH)3(C2O4) .2(C4H12N) .5(C6H13NO)' _chemical_formula_sum 'C85 H107 N7 O42 Zn9' _chemical_formula_weight 2487.47 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 orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 17.441(5) _cell_length_b 35.188(5) _cell_length_c 17.398(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 10677(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5586 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3848 _exptl_absorpt_coefficient_mu 2.048 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6614 _exptl_absorpt_correction_T_max 0.7352 _exptl_absorpt_process_details '(SADABS; Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex2 CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 52482 _diffrn_reflns_av_R_equivalents 0.0765 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 25.14 _reflns_number_total 9710 _reflns_number_gt 6277 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 'SHELXTL and local programs' _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^)+(0.1065P)^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 9710 _refine_ls_number_parameters 489 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1672 _refine_ls_wR_factor_gt 0.1557 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.951 _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 0.95740(9) 0.2500 0.61969(9) 0.0800(4) Uani 1 2 d S . . Zn2 Zn 0.79949(4) 0.203540(17) 0.58114(4) 0.02961(18) Uani 1 1 d . . . Zn3 Zn 0.80261(3) 0.086729(17) 0.17906(3) 0.02649(17) Uani 1 1 d . . . Zn4 Zn 0.81468(4) 0.128661(17) 0.01275(4) 0.02772(18) Uani 1 1 d . . . Zn5 Zn 0.86511(4) 0.036084(18) 0.02641(4) 0.03187(19) Uani 1 1 d . . . O1 O 0.9747(4) 0.2011(3) 0.5534(4) 0.167(4) Uani 1 1 d . . . O2 O 0.8664(2) 0.19242(13) 0.4948(2) 0.0462(11) Uani 1 1 d . . . O3 O 1.2070(2) 0.13473(13) 0.4554(3) 0.0464(11) Uani 1 1 d . . . O4 O 1.2023(2) 0.11003(13) 0.3378(2) 0.0456(11) Uani 1 1 d . . . O5 O 0.9564(3) 0.0927(2) 0.2091(3) 0.102(3) Uani 1 1 d . . . O6 O 0.8506(2) 0.11388(12) 0.2626(2) 0.0441(11) Uani 1 1 d . . . O7 O 0.8520(2) 0.18007(12) 0.0160(3) 0.0531(12) Uani 1 1 d . . . O8 O 0.9581(3) 0.14881(14) 0.0069(4) 0.095(2) Uani 1 1 d . . . O9 O 1.1994(2) 0.28136(11) -0.0409(3) 0.0494(12) Uani 1 1 d . . . O10 O 0.8075(3) 0.10869(11) -0.0912(2) 0.0487(12) Uani 1 1 d . . . O11 O 0.8143(3) 0.04571(12) -0.0733(2) 0.0493(12) Uani 1 1 d . . . O12 O 0.7870(3) 0.01034(12) 0.0943(2) 0.0567(13) Uani 1 1 d . . . O13 O 0.7790(3) 0.03532(11) 0.2113(2) 0.0455(11) Uani 1 1 d . . . O14 O 0.7459(4) 0.12762(13) 0.5559(3) 0.0763(18) Uani 1 1 d . . . O15 O 0.7899(3) 0.16169(11) 0.6535(2) 0.0492(12) Uani 1 1 d . . . O16 O 0.8378(3) 0.2500 0.6333(3) 0.0361(14) Uani 1 2 d S . . O17 O 0.9805(3) 0.04725(13) 0.0222(3) 0.0705(16) Uani 1 1 d . . . O18 O 1.0932(2) 0.01784(12) 0.0064(3) 0.0543(13) Uani 1 1 d . . . O19 O 0.85700(19) 0.08879(9) 0.0798(2) 0.0270(8) Uani 1 1 d . . . O20 O 1.037(2) 0.2500 0.683(2) 0.34(2) Uani 0.70 2 d SPU . . O20' O 0.960(2) 0.2889(13) 0.695(2) 0.25(2) Uani 0.30 1 d PU . . C1 C 0.9370(4) 0.1878(2) 0.5013(4) 0.060(2) Uani 1 1 d . . . C2 C 1.1727(3) 0.12579(16) 0.3940(3) 0.0321(13) Uani 1 1 d . . . C3 C 0.9222(4) 0.10985(19) 0.2610(4) 0.0474(17) Uani 1 1 d . . . C4 C 0.9749(3) 0.1639(2) 0.4405(4) 0.0446(17) Uani 1 1 d . . . C5 C 1.0528(3) 0.15640(18) 0.4463(4) 0.0418(16) Uani 1 1 d . . . H5 H 1.0805 0.1658 0.4878 0.050 Uiso 1 1 calc R . . C6 C 1.0900(3) 0.13482(17) 0.3900(3) 0.0354(14) Uani 1 1 d . . . C7 C 1.0459(3) 0.12035(18) 0.3288(3) 0.0396(15) Uani 1 1 d . . . H7 H 1.0695 0.1066 0.2899 0.048 Uiso 1 1 calc R . . C8 C 0.9676(3) 0.12647(19) 0.3262(4) 0.0421(16) Uani 1 1 d . . . C9 C 0.9332(3) 0.14831(18) 0.3818(3) 0.0402(15) Uani 1 1 d . . . H9 H 0.8807 0.1526 0.3795 0.048 Uiso 1 1 calc R . . C10 C 0.9241(4) 0.17883(18) 0.0102(4) 0.0490(17) Uani 1 1 d . . . C11 C 1.1679(5) 0.2500 -0.0351(5) 0.037(2) Uani 1 2 d S . . C12 C 0.9268(5) 0.2500 0.0123(5) 0.044(2) Uani 1 2 d S . . H12 H 0.8744 0.2500 0.0222 0.052 Uiso 1 2 calc SR . . C13 C 0.9669(3) 0.21563(16) 0.0047(4) 0.0448(16) Uani 1 1 d . . . C14 C 1.0451(3) 0.21630(16) -0.0076(4) 0.0429(16) Uani 1 1 d . . . H14 H 1.0720 0.1935 -0.0099 0.051 Uiso 1 1 calc R . . C15 C 1.0840(5) 0.2500 -0.0165(6) 0.043(2) Uani 1 2 d S . . C16 C 0.8023(3) 0.07580(17) -0.1130(3) 0.0350(14) Uani 1 1 d . . . C17 C 0.7753(4) 0.00832(16) 0.1652(3) 0.0391(15) Uani 1 1 d . . . C18 C 0.7667(4) 0.13066(17) 0.6236(4) 0.0510(18) Uani 1 1 d . . . C19 C 0.7667(4) 0.09753(16) 0.6763(4) 0.0437(16) Uani 1 1 d . . . C20 C 0.7465(4) 0.06140(17) 0.6485(4) 0.0488(18) Uani 1 1 d . . . H20 H 0.7337 0.0584 0.5969 0.059 Uiso 1 1 calc R . . C21 C 0.7454(4) 0.03002(15) 0.6972(3) 0.0413(16) Uani 1 1 d . . . C22 C 0.7642(4) 0.03443(15) 0.7726(3) 0.0366(14) Uani 1 1 d . . . H22 H 0.7641 0.0133 0.8047 0.044 Uiso 1 1 calc R . . C23 C 0.7836(3) 0.06987(16) 0.8029(3) 0.0353(14) Uani 1 1 d . . . C24 C 0.7836(4) 0.10098(15) 0.7539(3) 0.0368(14) Uani 1 1 d . . . H24 H 0.7953 0.1249 0.7736 0.044 Uiso 1 1 calc R . . C25 C 1.0207(4) 0.01898(18) 0.0094(4) 0.0484(17) Uani 1 1 d . . . C27 C 0.7260(7) 0.0732(3) 0.3837(6) 0.113(4) Uani 1 1 d . . . H27A H 0.7490 0.0951 0.3590 0.135 Uiso 1 1 calc R . . H27B H 0.7000 0.0584 0.3446 0.135 Uiso 1 1 calc R . . C28 C 0.7916(6) 0.0479(3) 0.4224(7) 0.122(4) Uani 1 1 d . . . H28A H 0.8276 0.0642 0.4481 0.183 Uiso 1 1 calc R . . H28B H 0.8177 0.0336 0.3834 0.183 Uiso 1 1 calc R . . H28C H 0.7690 0.0309 0.4589 0.183 Uiso 1 1 calc R . . C29 C 0.6105(6) 0.1104(3) 0.4074(6) 0.099(3) Uani 1 1 d . . . H29A H 0.5722 0.1170 0.4456 0.119 Uiso 1 1 calc R . . H29B H 0.5852 0.0968 0.3662 0.119 Uiso 1 1 calc R . . C30 C 0.6467(9) 0.1467(3) 0.3757(6) 0.155(6) Uani 1 1 d . . . H30A H 0.6838 0.1561 0.4117 0.232 Uiso 1 1 calc R . . H30B H 0.6076 0.1655 0.3677 0.232 Uiso 1 1 calc R . . H30C H 0.6716 0.1412 0.3277 0.232 Uiso 1 1 calc R . . N1 N 0.6693(4) 0.08617(19) 0.4422(4) 0.076(2) Uani 1 1 d . . . H1A H 0.6467 0.0658 0.4640 0.092 Uiso 1 1 calc R . . H1B H 0.6937 0.0992 0.4794 0.092 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 0.0761(10) 0.0784(10) 0.0855(10) 0.000 -0.0007(8) 0.000 Zn2 0.0293(4) 0.0192(3) 0.0404(4) 0.0001(3) 0.0053(3) 0.0027(3) Zn3 0.0283(4) 0.0242(3) 0.0270(3) -0.0013(2) -0.0034(3) 0.0014(3) Zn4 0.0285(4) 0.0224(3) 0.0324(4) 0.0006(3) 0.0060(3) -0.0023(3) Zn5 0.0336(4) 0.0267(4) 0.0353(4) -0.0025(3) 0.0038(3) 0.0041(3) O1 0.055(4) 0.305(11) 0.141(6) -0.170(7) -0.034(4) 0.073(5) O2 0.034(2) 0.062(3) 0.043(3) -0.010(2) 0.006(2) 0.005(2) O3 0.022(2) 0.063(3) 0.054(3) -0.016(2) -0.004(2) 0.003(2) O4 0.022(2) 0.068(3) 0.047(3) -0.017(2) -0.0003(19) 0.009(2) O5 0.047(3) 0.174(7) 0.086(4) -0.094(4) -0.025(3) 0.030(4) O6 0.021(2) 0.061(3) 0.051(3) -0.022(2) -0.0050(19) -0.004(2) O7 0.033(3) 0.034(3) 0.093(4) -0.005(2) 0.002(2) -0.009(2) O8 0.049(3) 0.026(3) 0.208(7) 0.005(3) 0.035(4) -0.004(2) O9 0.031(2) 0.024(2) 0.094(4) -0.007(2) 0.006(2) -0.0032(19) O10 0.085(4) 0.028(2) 0.034(2) -0.0055(19) 0.000(2) -0.011(2) O11 0.076(3) 0.031(2) 0.041(2) 0.005(2) -0.016(2) -0.005(2) O12 0.093(4) 0.036(3) 0.041(3) -0.001(2) 0.014(3) -0.025(2) O13 0.078(3) 0.022(2) 0.037(2) -0.0051(18) 0.011(2) -0.004(2) O14 0.152(6) 0.038(3) 0.039(3) 0.012(2) -0.037(3) -0.026(3) O15 0.086(3) 0.021(2) 0.041(2) 0.0015(18) -0.011(2) -0.008(2) O16 0.039(3) 0.015(3) 0.054(4) 0.000 -0.012(3) 0.000 O17 0.033(3) 0.038(3) 0.140(5) -0.036(3) 0.004(3) 0.009(2) O18 0.027(2) 0.040(3) 0.096(4) -0.018(2) 0.005(2) 0.004(2) O19 0.0235(19) 0.0188(19) 0.039(2) -0.0034(16) 0.0009(17) 0.0008(15) O20 0.31(4) 0.36(4) 0.34(4) 0.000 -0.26(3) 0.000 O20' 0.16(3) 0.31(5) 0.29(4) -0.24(4) -0.04(3) 0.04(3) C1 0.032(4) 0.095(6) 0.051(4) -0.042(4) -0.009(3) 0.024(4) C2 0.027(3) 0.037(3) 0.033(3) -0.005(3) 0.001(3) -0.003(3) C3 0.045(4) 0.050(4) 0.047(4) -0.019(3) -0.011(3) 0.002(3) C4 0.024(3) 0.066(5) 0.044(4) -0.017(3) -0.007(3) 0.008(3) C5 0.017(3) 0.061(4) 0.047(4) -0.027(3) -0.007(3) 0.004(3) C6 0.019(3) 0.046(4) 0.042(3) -0.014(3) -0.004(3) -0.003(3) C7 0.024(3) 0.056(4) 0.039(3) -0.015(3) -0.004(3) 0.008(3) C8 0.025(3) 0.055(4) 0.046(4) -0.013(3) -0.009(3) -0.004(3) C9 0.014(3) 0.063(4) 0.044(4) -0.017(3) -0.005(3) 0.005(3) C10 0.039(4) 0.030(4) 0.078(5) -0.005(3) 0.013(4) -0.011(3) C11 0.028(4) 0.018(4) 0.065(6) 0.000 -0.001(4) 0.000 C12 0.029(5) 0.028(5) 0.073(7) 0.000 0.010(4) 0.000 C13 0.032(4) 0.021(3) 0.081(5) 0.003(3) 0.006(3) -0.003(3) C14 0.031(3) 0.016(3) 0.082(5) -0.001(3) 0.006(3) -0.006(2) C15 0.031(5) 0.023(4) 0.075(7) 0.000 0.004(5) 0.000 C16 0.040(4) 0.039(4) 0.026(3) 0.001(3) -0.006(3) -0.011(3) C17 0.058(4) 0.025(3) 0.034(4) 0.007(3) 0.016(3) 0.000(3) C18 0.077(5) 0.026(3) 0.049(4) 0.001(3) -0.008(4) -0.012(3) C19 0.061(4) 0.022(3) 0.047(4) 0.005(3) -0.013(3) -0.002(3) C20 0.073(5) 0.032(4) 0.041(4) 0.000(3) -0.025(4) -0.006(3) C21 0.064(4) 0.018(3) 0.042(4) 0.006(3) -0.021(3) -0.011(3) C22 0.057(4) 0.024(3) 0.029(3) 0.005(2) -0.009(3) -0.004(3) C23 0.045(4) 0.034(3) 0.028(3) 0.009(3) -0.011(3) -0.006(3) C24 0.059(4) 0.018(3) 0.033(3) -0.001(2) -0.006(3) -0.005(3) C25 0.042(4) 0.035(4) 0.068(5) -0.012(3) 0.007(3) 0.000(3) C27 0.145(10) 0.100(8) 0.093(8) -0.027(6) 0.062(8) -0.009(8) C28 0.107(9) 0.130(11) 0.130(10) -0.010(8) 0.026(8) 0.028(8) C29 0.073(7) 0.109(8) 0.116(8) 0.032(7) -0.001(6) 0.018(6) C30 0.244(17) 0.116(11) 0.105(9) 0.034(8) 0.039(10) 0.025(11) N1 0.081(5) 0.068(5) 0.081(5) -0.018(4) 0.005(4) -0.015(4) _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 O20 1.77(2) . ? Zn1 O20' 1.89(3) . ? Zn1 O20' 1.89(3) 8_565 ? Zn1 O1 2.094(7) . ? Zn1 O1 2.094(7) 8_565 ? Zn1 O16 2.099(6) . ? Zn2 O2 1.942(4) . ? Zn2 O15 1.945(4) . ? Zn2 O9 1.955(4) 3_455 ? Zn2 O16 1.986(3) . ? Zn3 O6 1.930(4) . ? Zn3 O13 1.938(4) . ? Zn3 O4 1.954(4) 6_556 ? Zn3 O19 1.972(4) . ? Zn4 O7 1.924(4) . ? Zn4 O10 1.944(4) . ? Zn4 O19 1.968(3) . ? Zn4 O3 1.969(4) 6_556 ? Zn5 O11 1.977(4) . ? Zn5 O12 2.018(4) . ? Zn5 O17 2.052(5) . ? Zn5 O19 2.079(3) . ? Zn5 O18 2.111(4) 5_755 ? O1 C1 1.213(8) . ? O2 C1 1.245(8) . ? O3 C2 1.264(6) . ? O3 Zn4 1.969(4) 6_656 ? O4 C2 1.238(6) . ? O4 Zn3 1.954(4) 6_656 ? O5 C3 1.240(8) . ? O6 C3 1.257(7) . ? O7 C10 1.261(8) . ? O8 C10 1.213(8) . ? O9 C11 1.237(5) . ? O9 Zn2 1.955(4) 3 ? O10 C16 1.221(7) . ? O11 C16 1.282(7) . ? O12 C17 1.251(7) . ? O13 C17 1.245(7) . ? O14 C18 1.237(7) . ? O15 C18 1.275(7) . ? O16 Zn2 1.986(3) 8_565 ? O17 C25 1.238(7) . ? O18 C25 1.265(8) . ? O18 Zn5 2.111(4) 5_755 ? C1 C4 1.505(8) . ? C2 C6 1.479(8) . ? C3 C8 1.502(8) . ? C4 C9 1.367(8) . ? C4 C5 1.388(8) . ? C5 C6 1.399(8) . ? C5 H5 0.9300 . ? C6 C7 1.409(7) . ? C7 C8 1.383(8) . ? C7 H7 0.9300 . ? C8 C9 1.373(8) . ? C9 H9 0.9300 . ? C10 C13 1.498(8) . ? C11 O9 1.237(5) 8_565 ? C11 C15 1.497(12) . ? C12 C13 1.403(7) . ? C12 C13 1.403(7) 8_565 ? C12 H12 0.9300 . ? C13 C14 1.381(8) . ? C14 C15 1.375(7) . ? C14 H14 0.9300 . ? C15 C14 1.375(7) 8_565 ? C16 C23 1.513(7) 1_554 ? C17 C21 1.503(7) 2_654 ? C18 C19 1.484(8) . ? C19 C24 1.386(8) . ? C19 C20 1.405(8) . ? C20 C21 1.392(8) . ? C20 H20 0.9300 . ? C21 C22 1.361(8) . ? C21 C17 1.503(7) 2_655 ? C22 C23 1.396(8) . ? C22 H22 0.9300 . ? C23 C24 1.388(7) . ? C23 C16 1.513(7) 1_556 ? C24 H24 0.9300 . ? C25 C25 1.554(12) 5_755 ? C27 N1 1.492(11) . ? C27 C28 1.596(14) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 N1 1.465(10) . ? C29 C30 1.526(13) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? 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 O20 Zn1 O20' 63.3(13) . . ? O20 Zn1 O20' 63.3(13) . 8_565 ? O20' Zn1 O20' 93(3) . 8_565 ? O20 Zn1 O1 103.3(8) . . ? O20' Zn1 O1 166.2(14) . . ? O20' Zn1 O1 77.4(17) 8_565 . ? O20 Zn1 O1 103.3(8) . 8_565 ? O20' Zn1 O1 77.4(17) . 8_565 ? O20' Zn1 O1 166.2(14) 8_565 8_565 ? O1 Zn1 O1 110.6(6) . 8_565 ? O20 Zn1 O16 135.0(15) . . ? O20' Zn1 O16 87.0(11) . . ? O20' Zn1 O16 87.0(11) 8_565 . ? O1 Zn1 O16 101.8(2) . . ? O1 Zn1 O16 101.8(2) 8_565 . ? O2 Zn2 O15 113.6(2) . . ? O2 Zn2 O9 108.34(19) . 3_455 ? O15 Zn2 O9 111.15(19) . 3_455 ? O2 Zn2 O16 108.5(2) . . ? O15 Zn2 O16 110.89(19) . . ? O9 Zn2 O16 103.92(18) 3_455 . ? O6 Zn3 O13 109.65(18) . . ? O6 Zn3 O4 107.06(18) . 6_556 ? O13 Zn3 O4 104.17(19) . 6_556 ? O6 Zn3 O19 115.65(16) . . ? O13 Zn3 O19 112.95(15) . . ? O4 Zn3 O19 106.49(16) 6_556 . ? O7 Zn4 O10 112.91(19) . . ? O7 Zn4 O19 121.73(17) . . ? O10 Zn4 O19 108.50(16) . . ? O7 Zn4 O3 102.27(19) . 6_556 ? O10 Zn4 O3 103.87(19) . 6_556 ? O19 Zn4 O3 105.57(16) . 6_556 ? O11 Zn5 O12 106.7(2) . . ? O11 Zn5 O17 112.1(2) . . ? O12 Zn5 O17 140.3(2) . . ? O11 Zn5 O19 102.02(16) . . ? O12 Zn5 O19 95.34(16) . . ? O17 Zn5 O19 84.94(15) . . ? O11 Zn5 O18 94.12(18) . 5_755 ? O12 Zn5 O18 89.27(18) . 5_755 ? O17 Zn5 O18 79.89(17) . 5_755 ? O19 Zn5 O18 161.10(16) . 5_755 ? C1 O1 Zn1 130.5(6) . . ? C1 O2 Zn2 123.4(4) . . ? C2 O3 Zn4 131.4(4) . 6_656 ? C2 O4 Zn3 132.8(4) . 6_656 ? C3 O6 Zn3 111.0(4) . . ? C10 O7 Zn4 107.6(4) . . ? C11 O9 Zn2 131.9(5) . 3 ? C16 O10 Zn4 129.5(4) . . ? C16 O11 Zn5 133.4(4) . . ? C17 O12 Zn5 135.4(4) . . ? C17 O13 Zn3 122.4(4) . . ? C18 O15 Zn2 114.3(4) . . ? Zn2 O16 Zn2 110.8(3) . 8_565 ? Zn2 O16 Zn1 106.43(19) . . ? Zn2 O16 Zn1 106.43(19) 8_565 . ? C25 O17 Zn5 114.1(4) . . ? C25 O18 Zn5 112.6(4) . 5_755 ? Zn4 O19 Zn3 111.40(16) . . ? Zn4 O19 Zn5 113.39(17) . . ? Zn3 O19 Zn5 113.03(16) . . ? O1 C1 O2 123.6(6) . . ? O1 C1 C4 120.1(6) . . ? O2 C1 C4 116.3(6) . . ? O4 C2 O3 125.6(5) . . ? O4 C2 C6 117.8(5) . . ? O3 C2 C6 116.6(5) . . ? O5 C3 O6 123.3(6) . . ? O5 C3 C8 119.1(6) . . ? O6 C3 C8 117.6(6) . . ? C9 C4 C5 119.9(6) . . ? C9 C4 C1 121.0(5) . . ? C5 C4 C1 119.0(5) . . ? C4 C5 C6 120.4(5) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C7 118.1(5) . . ? C5 C6 C2 122.4(5) . . ? C7 C6 C2 119.4(5) . . ? C8 C7 C6 120.5(5) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C9 C8 C7 119.7(5) . . ? C9 C8 C3 121.3(5) . . ? C7 C8 C3 119.0(6) . . ? C4 C9 C8 121.2(5) . . ? C4 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? O8 C10 O7 121.4(6) . . ? O8 C10 C13 120.4(6) . . ? O7 C10 C13 118.2(6) . . ? O9 C11 O9 126.3(8) 8_565 . ? O9 C11 C15 116.8(4) 8_565 . ? O9 C11 C15 116.8(4) . . ? C13 C12 C13 119.1(8) . 8_565 ? C13 C12 H12 120.4 . . ? C13 C12 H12 120.4 8_565 . ? C14 C13 C12 119.5(6) . . ? C14 C13 C10 121.1(6) . . ? C12 C13 C10 119.4(6) . . ? C15 C14 C13 121.3(6) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C14 119.1(8) . 8_565 ? C14 C15 C11 120.4(4) . . ? C14 C15 C11 120.4(4) 8_565 . ? O10 C16 O11 127.1(5) . . ? O10 C16 C23 116.6(5) . 1_554 ? O11 C16 C23 116.3(5) . 1_554 ? O13 C17 O12 125.7(5) . . ? O13 C17 C21 117.3(5) . 2_654 ? O12 C17 C21 117.1(5) . 2_654 ? O14 C18 O15 123.8(6) . . ? O14 C18 C19 121.4(6) . . ? O15 C18 C19 114.8(6) . . ? C24 C19 C20 117.9(5) . . ? C24 C19 C18 122.2(5) . . ? C20 C19 C18 119.8(6) . . ? C21 C20 C19 120.8(6) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C21 C20 119.5(5) . . ? C22 C21 C17 121.2(5) . 2_655 ? C20 C21 C17 119.3(5) . 2_655 ? C21 C22 C23 121.7(5) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C24 C23 C22 118.2(5) . . ? C24 C23 C16 119.0(5) . 1_556 ? C22 C23 C16 122.8(5) . 1_556 ? C19 C24 C23 121.9(5) . . ? C19 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? O17 C25 O18 126.8(6) . . ? O17 C25 C25 117.7(7) . 5_755 ? O18 C25 C25 115.4(7) . 5_755 ? N1 C27 C28 111.0(9) . . ? N1 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? N1 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N1 C29 C30 110.3(9) . . ? N1 C29 H29A 109.6 . . ? C30 C29 H29A 109.6 . . ? N1 C29 H29B 109.6 . . ? C30 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 N1 C27 111.1(8) . . ? C29 N1 H1A 109.4 . . ? C27 N1 H1A 109.4 . . ? C29 N1 H1B 109.4 . . ? C27 N1 H1B 109.4 . . ? H1A N1 H1B 108.0 . . ? 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 O20 Zn1 O1 C1 -179.7(16) . . . . ? O20' Zn1 O1 C1 167(6) . . . . ? O20' Zn1 O1 C1 122.0(16) 8_565 . . . ? O1 Zn1 O1 C1 -69.7(12) 8_565 . . . ? O16 Zn1 O1 C1 37.9(11) . . . . ? O15 Zn2 O2 C1 -67.6(6) . . . . ? O9 Zn2 O2 C1 168.4(6) 3_455 . . . ? O16 Zn2 O2 C1 56.1(6) . . . . ? O13 Zn3 O6 C3 89.4(5) . . . . ? O4 Zn3 O6 C3 -158.1(5) 6_556 . . . ? O19 Zn3 O6 C3 -39.7(5) . . . . ? O10 Zn4 O7 C10 -80.8(5) . . . . ? O19 Zn4 O7 C10 51.0(5) . . . . ? O3 Zn4 O7 C10 168.2(5) 6_556 . . . ? O7 Zn4 O10 C16 162.5(5) . . . . ? O19 Zn4 O10 C16 24.5(6) . . . . ? O3 Zn4 O10 C16 -87.5(6) 6_556 . . . ? O12 Zn5 O11 C16 123.1(6) . . . . ? O17 Zn5 O11 C16 -65.7(6) . . . . ? O19 Zn5 O11 C16 23.7(6) . . . . ? O18 Zn5 O11 C16 -146.4(6) 5_755 . . . ? O11 Zn5 O12 C17 -152.4(6) . . . . ? O17 Zn5 O12 C17 40.3(8) . . . . ? O19 Zn5 O12 C17 -48.2(6) . . . . ? O18 Zn5 O12 C17 113.5(6) 5_755 . . . ? O6 Zn3 O13 C17 -152.5(5) . . . . ? O4 Zn3 O13 C17 93.2(5) 6_556 . . . ? O19 Zn3 O13 C17 -21.9(6) . . . . ? O2 Zn2 O15 C18 -56.4(5) . . . . ? O9 Zn2 O15 C18 66.1(5) 3_455 . . . ? O16 Zn2 O15 C18 -178.9(5) . . . . ? O2 Zn2 O16 Zn2 83.7(3) . . . 8_565 ? O15 Zn2 O16 Zn2 -151.0(2) . . . 8_565 ? O9 Zn2 O16 Zn2 -31.5(3) 3_455 . . 8_565 ? O2 Zn2 O16 Zn1 -31.7(3) . . . . ? O15 Zn2 O16 Zn1 93.7(3) . . . . ? O9 Zn2 O16 Zn1 -146.8(2) 3_455 . . . ? O20 Zn1 O16 Zn2 -120.86(18) . . . . ? O20' Zn1 O16 Zn2 -167.3(17) . . . . ? O20' Zn1 O16 Zn2 -74.4(17) 8_565 . . . ? O1 Zn1 O16 Zn2 2.0(4) . . . . ? O1 Zn1 O16 Zn2 116.3(3) 8_565 . . . ? O20 Zn1 O16 Zn2 120.86(18) . . . 8_565 ? O20' Zn1 O16 Zn2 74.4(17) . . . 8_565 ? O20' Zn1 O16 Zn2 167.3(17) 8_565 . . 8_565 ? O1 Zn1 O16 Zn2 -116.3(3) . . . 8_565 ? O1 Zn1 O16 Zn2 -2.0(4) 8_565 . . 8_565 ? O11 Zn5 O17 C25 -95.4(6) . . . . ? O12 Zn5 O17 C25 71.4(6) . . . . ? O19 Zn5 O17 C25 163.6(6) . . . . ? O18 Zn5 O17 C25 -5.1(5) 5_755 . . . ? O7 Zn4 O19 Zn3 88.5(2) . . . . ? O10 Zn4 O19 Zn3 -137.88(19) . . . . ? O3 Zn4 O19 Zn3 -27.1(2) 6_556 . . . ? O7 Zn4 O19 Zn5 -142.64(19) . . . . ? O10 Zn4 O19 Zn5 -9.0(2) . . . . ? O3 Zn4 O19 Zn5 101.8(2) 6_556 . . . ? O6 Zn3 O19 Zn4 -96.7(2) . . . . ? O13 Zn3 O19 Zn4 135.82(19) . . . . ? O4 Zn3 O19 Zn4 22.1(2) 6_556 . . . ? O6 Zn3 O19 Zn5 134.26(19) . . . . ? O13 Zn3 O19 Zn5 6.8(2) . . . . ? O4 Zn3 O19 Zn5 -107.0(2) 6_556 . . . ? O11 Zn5 O19 Zn4 -6.0(2) . . . . ? O12 Zn5 O19 Zn4 -114.3(2) . . . . ? O17 Zn5 O19 Zn4 105.6(2) . . . . ? O18 Zn5 O19 Zn4 142.1(5) 5_755 . . . ? O11 Zn5 O19 Zn3 122.0(2) . . . . ? O12 Zn5 O19 Zn3 13.7(2) . . . . ? O17 Zn5 O19 Zn3 -126.4(2) . . . . ? O18 Zn5 O19 Zn3 -89.9(5) 5_755 . . . ? Zn1 O1 C1 O2 -28.3(17) . . . . ? Zn1 O1 C1 C4 152.7(7) . . . . ? Zn2 O2 C1 O1 -24.4(14) . . . . ? Zn2 O2 C1 C4 154.6(5) . . . . ? Zn3 O4 C2 O3 9.2(10) 6_656 . . . ? Zn3 O4 C2 C6 -170.4(4) 6_656 . . . ? Zn4 O3 C2 O4 0.5(10) 6_656 . . . ? Zn4 O3 C2 C6 -179.9(4) 6_656 . . . ? Zn3 O6 C3 O5 4.6(10) . . . . ? Zn3 O6 C3 C8 -174.9(5) . . . . ? O1 C1 C4 C9 179.2(9) . . . . ? O2 C1 C4 C9 0.2(12) . . . . ? O1 C1 C4 C5 1.6(13) . . . . ? O2 C1 C4 C5 -177.4(7) . . . . ? C9 C4 C5 C6 3.6(11) . . . . ? C1 C4 C5 C6 -178.8(7) . . . . ? C4 C5 C6 C7 -1.4(10) . . . . ? C4 C5 C6 C2 -179.3(6) . . . . ? O4 C2 C6 C5 -172.5(6) . . . . ? O3 C2 C6 C5 8.0(9) . . . . ? O4 C2 C6 C7 9.6(9) . . . . ? O3 C2 C6 C7 -170.0(6) . . . . ? C5 C6 C7 C8 -2.0(10) . . . . ? C2 C6 C7 C8 176.1(6) . . . . ? C6 C7 C8 C9 3.1(10) . . . . ? C6 C7 C8 C3 -178.6(6) . . . . ? O5 C3 C8 C9 174.6(7) . . . . ? O6 C3 C8 C9 -5.9(10) . . . . ? O5 C3 C8 C7 -3.7(11) . . . . ? O6 C3 C8 C7 175.8(6) . . . . ? C5 C4 C9 C8 -2.5(11) . . . . ? C1 C4 C9 C8 179.9(7) . . . . ? C7 C8 C9 C4 -0.8(11) . . . . ? C3 C8 C9 C4 -179.1(6) . . . . ? Zn4 O7 C10 O8 -2.8(9) . . . . ? Zn4 O7 C10 C13 175.0(5) . . . . ? Zn2 O9 C11 O9 15.1(15) 3 . . 8_565 ? Zn2 O9 C11 C15 -167.4(6) 3 . . . ? C13 C12 C13 C14 2.1(14) 8_565 . . . ? C13 C12 C13 C10 -178.1(6) 8_565 . . . ? O8 C10 C13 C14 2.8(11) . . . . ? O7 C10 C13 C14 -175.0(7) . . . . ? O8 C10 C13 C12 -177.0(8) . . . . ? O7 C10 C13 C12 5.1(11) . . . . ? C12 C13 C14 C15 -3.4(12) . . . . ? C10 C13 C14 C15 176.7(7) . . . . ? C13 C14 C15 C14 4.7(14) . . . 8_565 ? C13 C14 C15 C11 -175.8(8) . . . . ? O9 C11 C15 C14 -0.9(13) 8_565 . . . ? O9 C11 C15 C14 -178.6(8) . . . . ? O9 C11 C15 C14 178.6(8) 8_565 . . 8_565 ? O9 C11 C15 C14 0.9(13) . . . 8_565 ? Zn4 O10 C16 O11 -13.8(10) . . . . ? Zn4 O10 C16 C23 169.4(4) . . . 1_554 ? Zn5 O11 C16 O10 -15.5(10) . . . . ? Zn5 O11 C16 C23 161.3(4) . . . 1_554 ? Zn3 O13 C17 O12 1.0(10) . . . . ? Zn3 O13 C17 C21 -178.6(4) . . . 2_654 ? Zn5 O12 C17 O13 43.3(11) . . . . ? Zn5 O12 C17 C21 -137.1(5) . . . 2_654 ? Zn2 O15 C18 O14 -5.7(10) . . . . ? Zn2 O15 C18 C19 174.0(5) . . . . ? O14 C18 C19 C24 -174.4(7) . . . . ? O15 C18 C19 C24 5.9(10) . . . . ? O14 C18 C19 C20 3.3(11) . . . . ? O15 C18 C19 C20 -176.4(7) . . . . ? C24 C19 C20 C21 -1.5(11) . . . . ? C18 C19 C20 C21 -179.3(7) . . . . ? C19 C20 C21 C22 -0.1(11) . . . . ? C19 C20 C21 C17 -179.1(6) . . . 2_655 ? C20 C21 C22 C23 1.0(11) . . . . ? C17 C21 C22 C23 179.9(6) 2_655 . . . ? C21 C22 C23 C24 -0.2(10) . . . . ? C21 C22 C23 C16 178.0(6) . . . 1_556 ? C20 C19 C24 C23 2.3(10) . . . . ? C18 C19 C24 C23 -179.9(6) . . . . ? C22 C23 C24 C19 -1.5(10) . . . . ? C16 C23 C24 C19 -179.8(6) 1_556 . . . ? Zn5 O17 C25 O18 -177.6(6) . . . . ? Zn5 O17 C25 C25 5.9(10) . . . 5_755 ? Zn5 O18 C25 O17 -175.2(6) 5_755 . . . ? Zn5 O18 C25 C25 1.3(10) 5_755 . . 5_755 ? C30 C29 N1 C27 -63.5(11) . . . . ? C28 C27 N1 C29 178.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.14 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.667 _refine_diff_density_min -2.758 _refine_diff_density_rms 0.120 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.080 -0.057 0.415 5064 1491 ' ' _platon_squeeze_details ; ;