# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name S.Telfer _publ_contact_author_address ; PO Box 11 222 Palmerston North 4442 ; _publ_contact_author_email s.telfer@massey.ac.nz loop_ _publ_author_name S.Telfer G.Waterhouse R.Deshpande G.Jameson # Attachment '- ms38 X-ray structures.cif' data_[Zn4O(1)3] _database_code_depnum_ccdc_archive 'CCDC 826054' #TrackingRef '- ms38 X-ray structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H39 N3 O22 Zn4' _chemical_formula_weight 1451.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 '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-43m 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' _cell_length_a 17.2108(17) _cell_length_b 17.2108(17) _cell_length_c 17.2108(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5098.0(9) _cell_formula_units_Z 1 _cell_measurement_temperature 292(2) _cell_measurement_reflns_used 5863 _cell_measurement_theta_min 7.25 _cell_measurement_theta_max 71.8 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 734 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 292(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rigaku MM007 rotating anode' _diffrn_radiation_monochromator 'Rigaku VariMax-HF Confocal Optical System' _diffrn_measurement_device_type 'Rigaku Spider' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21493 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 7.28 _diffrn_reflns_theta_max 64.94 _reflns_number_total 1535 _reflns_number_gt 1332 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2005)' _computing_cell_refinement 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_data_reduction 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Analysis of the data with XPREP indicated that the space group was P43m (Rint = 0.044). All non-hydrogen atoms of the Zn4O cluster and the skeleton of biphenyl-4,4'-dicarboxylate ligand (comprising Zn1, O1, O2, C1, C2, C3, C4 and C5) were refined anisotropically. Analysis with Platon indicated that there were 495 electrons per unit cell in addition to the Zn4O cluster and the biphenyl-4,4'-dicarboxylate ligand skeleton, which is consistent with the requirement for three nitrobenzyloxy side chains (231 electrons), along with additional disordered DEF. These side-chains are staistically disordered over four sites. As the atoms of these side chains could not be located from the difference Fourier map, they were placed in calculated positions with chemically reasonable bond lengths and angles and conformation. The atomic positions and thermal parameters of this side chain were held fixed during the refinement (Ueq = 0.20, based on the thermal parameters of C2 - C5). Restraints were placed upon certain bond distances and angles within the biphenyl skeleton to keep them within chemically sensible values. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.014(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.6(2) _refine_ls_number_reflns 1535 _refine_ls_number_parameters 35 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1172 _refine_ls_R_factor_gt 0.1138 _refine_ls_wR_factor_ref 0.3304 _refine_ls_wR_factor_gt 0.3214 _refine_ls_goodness_of_fit_ref 1.464 _refine_ls_restrained_S_all 1.462 _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 0.56531(5) 0.43469(5) 0.43469(5) 0.0890(8) Uani 1 6 d S . . O1 O 0.5000 0.5000 0.5000 0.075(3) Uani 1 24 d S . . O2 O 0.5475(4) 0.4525(4) 0.3254(4) 0.137(3) Uani 1 2 d S . . C1 C 0.5000 0.5000 0.2900 0.111(3) Uani 1 4 d S . . C2 C 0.5000 0.5000 0.2040(6) 0.125(4) Uani 1 4 d SD . . C3 C 0.5493(3) 0.4507(3) 0.1639(6) 0.217(10) Uani 1 2 d SD . . H3 H 0.5823 0.4177 0.1911 0.261 Uiso 1 2 calc SR . . C4 C 0.5498(3) 0.4502(3) 0.0831(6) 0.229(11) Uani 1 2 d SD . . C5 C 0.5000 0.5000 0.0427(9) 0.199(12) Uani 1 4 d SD . . C13 C 0.7500 0.2500 -0.0817 0.200 Uiso 0.25 2 d SP . . H13 H 0.7490 0.2510 -0.1357 0.240 Uiso 0.25 2 calc SPR . . C16 C 0.7500 0.2500 0.0795 0.200 Uiso 0.25 2 d SP . . C14 C 0.8000 0.2000 -0.0440 0.200 Uiso 0.25 2 d SP . . H14 H 0.8319 0.1681 -0.0738 0.240 Uiso 0.25 2 calc SPR . . C12 C 0.7000 0.3000 -0.0389 0.200 Uiso 0.25 2 d SP . . H12 H 0.6667 0.3333 -0.0654 0.240 Uiso 0.25 2 calc SPR . . C11 C 0.7000 0.3000 0.0429 0.200 Uiso 0.25 2 d SP . . C15 C 0.8050 0.1950 0.0369 0.200 Uiso 0.25 2 d SP . . H15 H 0.8387 0.1613 0.0624 0.240 Uiso 0.25 2 calc SPR . . N10 N 0.7500 0.2500 0.1640 0.200 Uiso 0.25 2 d SP . . O10 O 0.8034 0.2423 0.1773 0.200 Uiso 0.125 1 d P . . O11 O 0.7636 0.3050 0.1974 0.200 Uiso 0.125 1 d P . . C10 C 0.6500 0.3500 0.0880 0.200 Uiso 0.25 2 d SP . . H10A H 0.6821 0.3823 0.1213 0.240 Uiso 0.125 1 calc PR . . H10B H 0.6177 0.3179 0.1213 0.240 Uiso 0.125 1 calc PR . . O12 O 0.6000 0.4000 0.0420 0.200 Uiso 0.25 2 d SP . . H4 H 0.5885 0.4115 0.0535 0.240 Uiso 0.75 2 d SP . . 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 0.0890(8) 0.0890(8) 0.0890(8) -0.0040(4) 0.0040(4) 0.0040(4) O1 0.075(3) 0.075(3) 0.075(3) 0.000 0.000 0.000 O2 0.170(4) 0.170(4) 0.071(3) -0.009(3) 0.009(3) -0.003(5) C1 0.127(6) 0.127(6) 0.078(7) 0.000 0.000 0.017(7) C2 0.155(7) 0.155(7) 0.065(6) 0.000 0.000 -0.024(9) C3 0.285(16) 0.285(16) 0.083(8) -0.012(6) 0.012(6) 0.09(2) C4 0.298(19) 0.298(19) 0.089(10) -0.002(6) 0.002(6) 0.08(2) C5 0.26(2) 0.26(2) 0.070(9) 0.000 0.000 -0.11(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 1.930(6) 7_665 ? Zn1 O2 1.930(6) . ? Zn1 O2 1.930(6) 8_656 ? Zn1 O1 1.9468(15) . ? O1 Zn1 1.9468(15) 3_566 ? O1 Zn1 1.9468(15) 4_656 ? O1 Zn1 1.9468(15) 2_665 ? O2 C1 1.307(9) . ? C1 O2 1.307(8) 2_665 ? C1 C2 1.480(11) . ? C2 C3 1.385(7) 13 ? C2 C3 1.385(7) . ? C3 C4 1.391(9) . ? C3 H3 0.9300 . ? C4 C5 1.396(7) . ? C4 O12 1.412(8) . ? C4 H4 1.072(8) . ? C5 C4 1.396(7) 13 ? C5 C5 1.47(3) 3_565 ? C13 C14 1.37897(13) . ? C13 C12 1.42272(14) . ? C13 H13 0.9300 . ? C16 C11 1.37061(14) . ? C16 N10 1.45511(14) . ? C16 C15 1.52646(15) . ? C16 O10 1.92188(19) . ? C16 O10 1.92188(19) 14_665 ? C14 C15 1.39727(14) . ? C14 H14 0.9300 . ? C12 C11 1.40659(14) . ? C12 H12 0.9300 . ? C11 C10 1.44384(14) . ? C15 H15 0.9300 . ? N10 O10 0.9565 . ? N10 O10 0.9565 14_665 ? N10 O11 1.13205(12) . ? N10 O11 1.13205(12) 14_665 ? N10 O10 1.37783(15) 24_656 ? N10 O10 1.37783(13) 8_656 ? N10 O11 1.80643(18) 24_656 ? N10 O11 1.80643(19) 8_656 ? O10 O10 0.4701 24_656 ? O10 O10 1.11284(12) 14_665 ? O10 O11 1.32464(13) . ? O10 N10 1.37783(14) 7_665 ? O10 O10 1.40804(14) 8_656 ? O10 O10 1.40804(15) 7_665 ? O10 O11 1.48323(15) 24_656 ? O10 O10 1.58296(16) 17 ? O11 O11 0.9472 24_656 ? O11 O10 1.48323(16) 24_656 ? O11 O11 1.67081(18) 14_665 ? O11 N10 1.80643(18) 7_665 ? C10 O12 1.45155(15) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O2 106.5(3) 7_665 . ? O2 Zn1 O2 106.5(3) 7_665 8_656 ? O2 Zn1 O2 106.5(3) . 8_656 ? O2 Zn1 O1 112.3(3) 7_665 . ? O2 Zn1 O1 112.3(3) . . ? O2 Zn1 O1 112.3(3) 8_656 . ? Zn1 O1 Zn1 109.5 3_566 4_656 ? Zn1 O1 Zn1 109.5 3_566 2_665 ? Zn1 O1 Zn1 109.5 4_656 2_665 ? Zn1 O1 Zn1 109.5 3_566 . ? Zn1 O1 Zn1 109.5 4_656 . ? Zn1 O1 Zn1 109.5 2_665 . ? C1 O2 Zn1 130.7(6) . . ? O2 C1 O2 124.5(7) . 2_665 ? O2 C1 C2 117.8(3) . . ? O2 C1 C2 117.8(3) 2_665 . ? C3 C2 C3 120.2(10) 13 . ? C3 C2 C1 119.9(5) 13 . ? C3 C2 C1 119.9(5) . . ? C2 C3 C4 120.4(8) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C4 C5 119.4(8) . . ? C3 C4 O12 120.4(6) . . ? C5 C4 O12 120.2(7) . . ? C3 C4 H4 118.8(7) . . ? C5 C4 H4 121.8(8) . . ? O12 C4 H4 1.65(13) . . ? C4 C5 C4 120.3(12) 13 . ? C4 C5 C5 119.9(6) 13 3_565 ? C4 C5 C5 119.9(6) . 3_565 ? C14 C13 C12 120.8 . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C11 C16 N10 117.4 . . ? C11 C16 C15 123.9 . . ? N10 C16 C15 118.7 . . ? C11 C16 O10 138.3 . . ? N10 C16 O10 28.9 . . ? C15 C16 O10 94.7 . . ? C11 C16 O10 138.3 . 14_665 ? N10 C16 O10 28.9 . 14_665 ? C15 C16 O10 94.7 . 14_665 ? O10 C16 O10 33.7 . 14_665 ? C13 C14 C15 123.0 . . ? C13 C14 H14 118.5 . . ? C15 C14 H14 118.5 . . ? C11 C12 C13 121.2 . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C16 C11 C12 117.4 . . ? C16 C11 C10 120.1 . . ? C12 C11 C10 122.6 . . ? C14 C15 C16 113.7 . . ? C14 C15 H15 123.1 . . ? C16 C15 H15 123.1 . . ? O10 N10 O10 71.143(1) . 14_665 ? O10 N10 O11 78.2 . . ? O10 N10 O11 130.9 14_665 . ? O10 N10 O11 130.9 . 14_665 ? O10 N10 O11 78.2 14_665 14_665 ? O11 N10 O11 95.1 . 14_665 ? O10 N10 O10 10.4 . 24_656 ? O10 N10 O10 71.629(1) 14_665 24_656 ? O11 N10 O10 71.7 . 24_656 ? O11 N10 O10 122.3 14_665 24_656 ? O10 N10 O10 71.6 . 8_656 ? O10 N10 O10 10.4 14_665 8_656 ? O11 N10 O10 122.3 . 8_656 ? O11 N10 O10 71.7 14_665 8_656 ? O10 N10 O10 70.1 24_656 8_656 ? O10 N10 C16 103.7 . . ? O10 N10 C16 103.7 14_665 . ? O11 N10 C16 120.5 . . ? O11 N10 C16 120.5 14_665 . ? O10 N10 C16 114.0 24_656 . ? O10 N10 C16 114.0 8_656 . ? O10 N10 O11 55.1 . 24_656 ? O10 N10 O11 105.7 14_665 24_656 ? O11 N10 O11 100.2 14_665 24_656 ? O10 N10 O11 46.8 24_656 24_656 ? O10 N10 O11 98.5 8_656 24_656 ? C16 N10 O11 133.5 . 24_656 ? O10 N10 O11 105.7 . 8_656 ? O10 N10 O11 55.1 14_665 8_656 ? O11 N10 O11 100.2 . 8_656 ? O10 N10 O11 98.5 24_656 8_656 ? O10 N10 O11 46.8 8_656 8_656 ? C16 N10 O11 133.5 . 8_656 ? O11 N10 O11 92.9 24_656 8_656 ? O10 O10 N10 147.975(1) 24_656 . ? O10 O10 O10 120.000(1) 24_656 14_665 ? N10 O10 O10 54.429(1) . 14_665 ? O10 O10 O11 100.4 24_656 . ? N10 O10 O11 56.8 . . ? O10 O10 O11 102.2 14_665 . ? N10 O10 N10 126.4 . 7_665 ? O10 O10 N10 110.8 14_665 7_665 ? O11 O10 N10 83.9 . 7_665 ? O10 O10 O10 103.193(1) 24_656 8_656 ? N10 O10 O10 68.2 . 8_656 ? O10 O10 O10 16.8 14_665 8_656 ? O11 O10 O10 107.3 . 8_656 ? N10 O10 O10 95.1 7_665 8_656 ? O10 O10 O10 43.2 24_656 7_665 ? N10 O10 O10 119.6 . 7_665 ? O10 O10 O10 76.807(1) 14_665 7_665 ? O11 O10 O10 111.6 . 7_665 ? O10 O10 O10 60.000(1) 8_656 7_665 ? O10 O10 O11 61.459(1) 24_656 24_656 ? N10 O10 O11 93.0 . 24_656 ? O10 O10 O11 120.5 14_665 24_656 ? N10 O10 O11 46.4 7_665 24_656 ? O10 O10 O11 114.3 8_656 24_656 ? O10 O10 O11 82.2 7_665 24_656 ? O10 O10 O10 60.0 24_656 17 ? N10 O10 O10 105.4 . 17 ? O10 O10 O10 60.0 14_665 17 ? O11 O10 O10 113.0 . 17 ? N10 O10 O10 54.9 7_665 17 ? O10 O10 O10 43.2 8_656 17 ? O11 O10 O10 91.7 24_656 17 ? O10 O10 C16 163.201(1) 24_656 . ? N10 O10 C16 47.3 . . ? O10 O10 C16 73.2 14_665 . ? O11 O10 C16 85.8 . . ? N10 O10 C16 169.5 7_665 . ? O10 O10 C16 89.7 8_656 . ? O10 O10 C16 147.9 7_665 . ? O11 O10 C16 123.0 24_656 . ? O10 O10 C16 131.9 17 . ? O11 O11 N10 120.4 24_656 . ? O11 O11 O10 79.6 24_656 . ? N10 O11 O10 45.0 . . ? O11 O11 O10 61.5 24_656 24_656 ? N10 O11 O10 61.9 . 24_656 ? O11 O11 O11 120.0 24_656 14_665 ? N10 O11 O11 42.4 . 14_665 ? O10 O11 O11 77.8 . 14_665 ? O10 O11 O11 88.3 24_656 14_665 ? O11 O11 N10 32.7 24_656 7_665 ? N10 O11 N10 87.6 . 7_665 ? O10 O11 N10 49.3 . 7_665 ? O11 O11 N10 96.7 14_665 7_665 ? C11 C10 O12 114.4 . . ? C11 C10 H10A 108.7 . . ? O12 C10 H10A 108.7 . . ? C11 C10 H10B 108.7 . . ? O12 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C4 O12 C10 117.0(4) . . ? C10 O12 H4 111.8 . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 64.94 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 0.573 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.082 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 -0.023 -0.010 -0.007 2820 305 ' ' _platon_squeeze_details ; SQUEEZE was used to account for the disordered solvent in the voids of this MOF. The number of electrons corresponds to approximately 5 DEF solvent molecules per unit cell. R1 was observed to drop from 0.247 to 0.121 and wR2 from 0.55 to 0.33. ; #END data_b-[Zn4O(3)3] _database_code_depnum_ccdc_archive 'CCDC 826055' #TrackingRef '- ms38 X-ray structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H30 O16 Zn4' _chemical_formula_weight 1088.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P-42(1)m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 17.2215(4) _cell_length_b 17.2215(4) _cell_length_c 17.1168(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5076.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 292(2) _cell_measurement_reflns_used 19505 _cell_measurement_theta_min 7.25 _cell_measurement_theta_max 62.38 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 1.343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.55 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 292(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rigaku MM007 rotating anode' _diffrn_radiation_monochromator 'Rigaku VariMax-HF Confocal Optical System' _diffrn_measurement_device_type 'Rigaku Spider' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38669 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 7.27 _diffrn_reflns_theta_max 62.37 _reflns_number_total 4241 _reflns_number_gt 3747 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2005)' _computing_cell_refinement 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_data_reduction 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. O225, C225, O207 and C207 were disordered with site occupancies of only 0.5, so were restricted to isotropic atomic displacement parameters. Very weak electron density was observed at the sites modelled; almost certainly the methoxy groups were disordered over another three crystallographically distinct sites in even lower occupancy; thus, the isotropic atomic displacement parameters for these atoms included in the model were constrained to 0.20. Electron density in large solvent voids was handled with SQUEEZE procedure of PLATON (vide infra). There are large librational motions about 1,4 vectors for each phenyl ring, which raises a host of A- and B-level alerts for high/low Ueq values compared to neighbouring atoms and leads in turn to alerts for foreshortening of bond distances. ; _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^)+(0.1718P)^2^+0.0925P] 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 0.44(9) _refine_ls_number_reflns 4241 _refine_ls_number_parameters 158 _refine_ls_number_restraints 121 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.2202 _refine_ls_wR_factor_gt 0.2125 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.157 _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 0.06538(3) 0.56538(3) 0.94481(4) 0.0708(3) Uani 1 2 d S . . Zn2 Zn 0.06563(3) 0.43437(3) 0.81561(4) 0.0742(3) Uani 1 2 d S . . O50 O 0.0000 0.5000 0.8810(2) 0.0616(12) Uani 1 4 d S . . O1 O 0.0525(4) 0.5525(4) 1.0558(3) 0.155(3) Uani 1 2 d S . . O10 O 0.0540(4) 0.4460(4) 0.7090(4) 0.177(3) Uani 1 2 d SU . . O20 O 0.0496(2) 0.67477(19) 0.9280(3) 0.1061(12) Uani 1 1 d . . . O21 O 0.0483 0.3254(2) 0.8423(4) 0.1335(17) Uani 1 1 d . . . C1 C 0.0000 0.5000 1.0914(8) 0.124(4) Uani 1 4 d SU . . C2 C 0.0000 0.5000 1.1718(9) 0.208(9) Uani 1 4 d SDU . . C3 C -0.0498(3) 0.4502(3) 1.2141(5) 0.175(5) Uani 1 2 d SDU . . H3 H -0.0831 0.4169 1.1876 0.210 Uiso 1 2 calc SR . . C4 C -0.0490(3) 0.4510(3) 1.2960(5) 0.170(5) Uani 1 2 d SDU . . H4 H -0.0823 0.4177 1.3225 0.204 Uiso 1 2 calc SR . . C5 C 0.0000 0.5000 1.3402(7) 0.164(7) Uani 1 4 d SDU . . C6 C 0.0000 0.5000 1.4215(7) 0.176(7) Uani 1 4 d SDU . . C7 C 0.04906(2) 0.45094(2) 1.4676(5) 0.216(7) Uani 1 2 d SDU . . C8 C 0.0502(5) 0.4498(5) 1.5492(5) 0.238(8) Uani 1 2 d SDU . . H8 H 0.0829 0.4171 1.5774 0.285 Uiso 1 2 calc SR . . C9 C 0.0000 0.5000 1.5847(10) 0.169(6) Uani 1 4 d SDU . . C10 C 0.0000 0.5000 0.6763(9) 0.147(5) Uani 1 4 d SU . . C20 C -0.0005(2) 0.7092(3) 0.8827(3) 0.0970(16) Uani 1 1 d U . . C21 C 0.0005(3) 0.7955(4) 0.8847(3) 0.119(2) Uani 1 1 d DU . . C22 C 0.0550(4) 0.8345(3) 0.9213(4) 0.135(2) Uani 1 1 d DU . . H22 H 0.0933 0.8079 0.9486 0.163 Uiso 1 1 calc R . . C23 C 0.0560(4) 0.9161(3) 0.9195(4) 0.150(3) Uani 1 1 d DU . . H23 H 0.0951 0.9426 0.9458 0.180 Uiso 1 1 calc R . . C24 C 0.0029(4) 0.9558(4) 0.8814(4) 0.140(3) Uani 1 1 d DU . . C25 C -0.0506(5) 0.9183(4) 0.8457(5) 0.218(5) Uani 1 1 d DU . . C26 C -0.0529(6) 0.8322(4) 0.8465(6) 0.254(6) Uani 1 1 d DU . . H26 H -0.0918 0.8053 0.8202 0.305 Uiso 1 1 calc R . . C207 C 0.1425 0.3575 1.4811 0.200 Uiso 0.50 2 d SP A 1 H20A H 0.1764 0.3236 1.4525 0.300 Uiso 0.50 2 calc SPR A 1 H20B H 0.1085 0.3272 1.5133 0.300 Uiso 0.25 1 calc PR A 1 H20C H 0.1728 0.3915 1.5133 0.300 Uiso 0.25 1 calc PR A 1 O207 O 0.0990 0.4010 1.4293 0.200 Uiso 0.50 2 d SP A 1 C225 C -0.1734 0.9179 0.7709 0.200 Uiso 0.50 1 d P B 1 H22A H -0.2100 0.9519 0.7460 0.300 Uiso 0.50 1 calc PR B 1 H22B H -0.1995 0.8875 0.8098 0.300 Uiso 0.50 1 calc PR B 1 H22C H -0.1507 0.8841 0.7326 0.300 Uiso 0.50 1 calc PR B 1 O225 O -0.1141 0.9627 0.8069 0.200 Uiso 0.50 1 d P B 1 H25 H -0.0921 0.9444 0.8216 0.200 Uiso 0.50 1 d P . . H7 H 0.0818 0.4182 1.4406 0.200 Uiso 0.50 2 d SP . . 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 0.0681(3) 0.0681(3) 0.0762(4) -0.0038(2) -0.0038(2) -0.0009(4) Zn2 0.0711(3) 0.0711(3) 0.0805(5) -0.0039(2) 0.0039(2) 0.0077(4) O50 0.0646(19) 0.0646(19) 0.056(2) 0.000 0.000 -0.0016(19) O1 0.200(5) 0.200(5) 0.065(3) 0.004(2) 0.004(2) -0.014(7) O10 0.220(5) 0.220(5) 0.091(3) 0.002(3) -0.002(3) 0.030(7) O20 0.109(3) 0.0667(18) 0.143(3) -0.0007(18) -0.012(2) 0.0057(18) O21 0.137(3) 0.077(2) 0.186(5) 0.015(2) 0.043(3) 0.013(2) C1 0.146(7) 0.146(7) 0.080(6) 0.000 0.000 -0.020(9) C2 0.270(14) 0.270(14) 0.083(8) 0.000 0.000 -0.044(18) C3 0.214(8) 0.214(8) 0.096(6) -0.002(5) -0.002(5) -0.029(11) C4 0.199(8) 0.199(8) 0.112(7) 0.021(5) 0.021(5) -0.033(10) C5 0.207(11) 0.207(11) 0.076(7) 0.000 0.000 0.038(13) C6 0.230(12) 0.230(12) 0.067(6) 0.000 0.000 -0.036(14) C7 0.284(11) 0.284(11) 0.079(5) -0.013(6) 0.013(6) 0.038(15) C8 0.315(13) 0.315(13) 0.082(5) 0.003(5) -0.003(5) 0.141(16) C9 0.199(8) 0.199(8) 0.110(8) 0.000 0.000 0.003(9) C10 0.170(7) 0.170(7) 0.100(6) 0.000 0.000 -0.003(8) C20 0.097(4) 0.068(3) 0.125(4) -0.011(2) 0.016(4) -0.0065(19) C21 0.124(5) 0.064(3) 0.168(6) 0.000(3) -0.003(5) 0.026(2) C22 0.136(5) 0.061(3) 0.210(7) -0.012(3) -0.010(5) 0.002(3) C23 0.186(7) 0.056(3) 0.208(7) -0.006(3) -0.027(6) -0.002(4) C24 0.179(8) 0.050(4) 0.191(8) -0.012(3) 0.011(7) -0.007(3) C25 0.249(11) 0.061(4) 0.342(13) 0.008(5) -0.111(10) 0.026(5) C26 0.296(11) 0.053(3) 0.413(15) -0.017(6) -0.178(11) -0.018(5) _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 1.925(3) 8_455 ? Zn1 O20 1.925(3) . ? Zn1 O1 1.925(5) . ? Zn1 O50 1.931(2) . ? Zn1 Zn2 3.1594(9) 2_565 ? Zn2 O10 1.847(7) . ? Zn2 O50 1.952(2) . ? Zn2 O21 1.954(4) . ? Zn2 O21 1.954(4) 7 ? Zn2 Zn1 3.1594(9) 2_565 ? O50 Zn1 1.931(2) 2_565 ? O50 Zn2 1.952(2) 2_565 ? O1 C1 1.417(10) . ? O10 C10 1.429(10) . ? O20 C20 1.302(6) . ? O21 C20 1.230(6) 2_565 ? C1 C2 1.38(2) . ? C1 O1 1.417(10) 2_565 ? C2 C3 1.412(8) 2_565 ? C2 C3 1.412(8) . ? C3 C4 1.402(8) . ? C3 H3 0.9300 . ? C4 C5 1.412(7) . ? C4 H4 0.9300 . ? C5 C6 1.392(19) . ? C5 C4 1.412(7) 2_565 ? C6 C7 1.432(6) 2_565 ? C6 C7 1.432(6) . ? C7 O207 1.382(4) . ? C7 C8 1.396(8) . ? C7 H7 0.923(4) . ? C8 C9 1.366(9) . ? C8 H8 0.9300 . ? C9 C8 1.366(9) 2_565 ? C9 C10 1.57(2) 1_556 ? C10 O10 1.429(10) 2_565 ? C10 C9 1.57(2) 1_554 ? C20 O21 1.230(6) 2_565 ? C20 C21 1.487(8) . ? C21 C26 1.294(11) . ? C21 C22 1.312(9) . ? C22 C23 1.406(8) . ? C22 H22 0.9300 . ? C23 C24 1.315(9) . ? C23 H23 0.9300 . ? C24 C25 1.280(11) . ? C24 C24 1.526(12) 2_575 ? C25 C26 1.483(9) . ? C25 O225 1.490(8) . ? C25 H25 0.939(8) . ? C26 H26 0.9300 . ? C207 O207 1.3812 . ? C207 H20A 0.9600 . ? C207 H20B 0.9600 . ? C207 H20C 0.9600 . ? O207 H7 0.4608 . ? C225 O225 1.4206 . ? C225 H22A 0.9600 . ? C225 H22B 0.9600 . ? C225 H22C 0.9600 . ? O225 H25 0.5536 . ? 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 104.8(2) 8_455 . ? O20 Zn1 O1 104.1(2) 8_455 . ? O20 Zn1 O1 104.1(2) . . ? O20 Zn1 O50 113.83(14) 8_455 . ? O20 Zn1 O50 113.83(14) . . ? O1 Zn1 O50 115.1(3) . . ? O20 Zn1 Zn2 126.49(15) 8_455 2_565 ? O20 Zn1 Zn2 78.07(13) . 2_565 ? O1 Zn1 Zn2 127.5(2) . 2_565 ? O50 Zn1 Zn2 35.76(5) . 2_565 ? O10 Zn2 O50 116.2(3) . . ? O10 Zn2 O21 108.6(3) . . ? O50 Zn2 O21 109.47(14) . . ? O10 Zn2 O21 108.6(3) . 7 ? O50 Zn2 O21 109.47(14) . 7 ? O21 Zn2 O21 103.85(12) . 7 ? O10 Zn2 Zn1 127.9(2) . 2_565 ? O50 Zn2 Zn1 35.31(5) . 2_565 ? O21 Zn2 Zn1 74.24(13) . 2_565 ? O21 Zn2 Zn1 121.47(19) 7 2_565 ? Zn1 O50 Zn1 111.15(19) . 2_565 ? Zn1 O50 Zn2 108.931(17) . . ? Zn1 O50 Zn2 108.931(17) 2_565 . ? Zn1 O50 Zn2 108.931(17) . 2_565 ? Zn1 O50 Zn2 108.931(17) 2_565 2_565 ? Zn2 O50 Zn2 109.96(19) . 2_565 ? C1 O1 Zn1 124.8(7) . . ? C10 O10 Zn2 121.9(8) . . ? C20 O20 Zn1 128.9(4) . . ? C20 O21 Zn2 134.4(4) 2_565 . ? C2 C1 O1 115.5(5) . 2_565 ? C2 C1 O1 115.5(5) . . ? O1 C1 O1 129.0(11) 2_565 . ? C1 C2 C3 120.9(6) . 2_565 ? C1 C2 C3 120.9(6) . . ? C3 C2 C3 118.3(12) 2_565 . ? C4 C3 C2 120.1(9) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 123.2(8) . . ? C3 C4 H4 118.4 . . ? C5 C4 H4 118.4 . . ? C6 C5 C4 122.4(5) . . ? C6 C5 C4 122.4(5) . 2_565 ? C4 C5 C4 115.2(10) . 2_565 ? C5 C6 C7 123.5(4) . 2_565 ? C5 C6 C7 123.5(4) . . ? C7 C6 C7 113.1(7) 2_565 . ? O207 C7 C8 117.2(5) . . ? O207 C7 C6 118.2(6) . . ? C8 C7 C6 124.6(6) . . ? O207 C7 H7 1.77(14) . . ? C8 C7 H7 119.0(6) . . ? C6 C7 H7 116.4(7) . . ? C9 C8 C7 115.2(12) . . ? C9 C8 H8 122.4 . . ? C7 C8 H8 122.4 . . ? C8 C9 C8 127.2(16) 2_565 . ? C8 C9 C10 116.4(8) 2_565 1_556 ? C8 C9 C10 116.4(8) . 1_556 ? O10 C10 O10 133.9(13) . 2_565 ? O10 C10 C9 113.0(7) . 1_554 ? O10 C10 C9 113.0(6) 2_565 1_554 ? O21 C20 O20 123.9(6) 2_565 . ? O21 C20 C21 120.4(5) 2_565 . ? O20 C20 C21 115.7(5) . . ? C26 C21 C22 120.0(7) . . ? C26 C21 C20 117.9(6) . . ? C22 C21 C20 122.1(5) . . ? C21 C22 C23 120.7(7) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 121.4(7) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C25 C24 C23 118.4(7) . . ? C25 C24 C24 117.2(7) . 2_575 ? C23 C24 C24 124.3(7) . 2_575 ? C24 C25 C26 121.3(8) . . ? C24 C25 O225 118.7(6) . . ? C26 C25 O225 119.9(8) . . ? C24 C25 H25 121.0(8) . . ? C26 C25 H25 117.5(9) . . ? O225 C25 H25 2.60(19) . . ? C21 C26 C25 118.3(8) . . ? C21 C26 H26 120.9 . . ? C25 C26 H26 120.9 . . ? O207 C207 H20A 109.5 . . ? O207 C207 H20B 109.5 . . ? H20A C207 H20B 109.5 . . ? O207 C207 H20C 109.5 . . ? H20A C207 H20C 109.5 . . ? H20B C207 H20C 109.5 . . ? C207 O207 C7 111.7(3) . . ? C207 O207 H7 115.291(2) . . ? C7 O207 H7 3.6(3) . . ? O225 C225 H22A 109.5 . . ? O225 C225 H22B 109.5 . . ? H22A C225 H22B 109.5 . . ? O225 C225 H22C 109.5 . . ? H22A C225 H22C 109.5 . . ? H22B C225 H22C 109.5 . . ? C225 O225 C25 116.2(3) . . ? C225 O225 H25 112.179(1) . . ? C25 O225 H25 4.4(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 62.37 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.522 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.069 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 0.152 0.291 0.081 3231 413 ' ' _platon_squeeze_details ; SQUEEZE was used to account for the disordered solvent in the voids of this MOF. The number of electrons corresponds to approximately 7 DEF solvent molecules per unit cell i.e. 3.5 molecules per formula unit. ;