# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Shuxia Liu' _publ_contact_author_address ; Department of Chemistry Institute of Polyoxometalate Chemistry Changchun 130024 CHINA ; _publ_contact_author_email LIUSX@NENU.EDU.CN _publ_section_title ; A three-dimensional porous metal-organic framework with the rutile topology constructed from triangular and distorted octahedral building blocks ; loop_ _publ_author_name 'Shuxia Liu' 'Bo Gao' 'Dehui Li' 'Zhongmin Su' 'Chunyan Sun' 'Linhua Xie' ; Chundan Zhang ; data_znbtc _database_code_depnum_ccdc_archive 'CCDC 258251' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H18 N2 O7 Zn' _chemical_formula_weight 391.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4550(6) _cell_length_b 16.0074(11) _cell_length_c 11.0347(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.4660(10) _cell_angle_gamma 90.00 _cell_volume 1651.90(19) _cell_formula_units_Z 4 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used 9962 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 1.525 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.584 _exptl_absorpt_correction_T_max 0.737 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3813 _diffrn_standards_interval_count 12.88 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9962 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 28.29 _reflns_number_total 3813 _reflns_number_gt 3005 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. ; _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^)+(0.0757P)^2^+0.0808P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3813 _refine_ls_number_parameters 227 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1265 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.073 _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 0.13113(3) 0.07995(2) 0.93129(3) 0.01765(13) Uani 1 1 d . . . O1 O 0.2030(2) -0.00498(17) 1.0554(2) 0.0357(6) Uani 1 1 d . . . O2 O -0.0457(2) 0.04746(15) 0.8253(2) 0.0257(5) Uani 1 1 d . . . O3 O 0.2944(2) 0.06788(13) 0.8452(2) 0.0231(5) Uani 1 1 d . . . O4 O 0.2177(2) 0.16975(15) 0.7147(2) 0.0282(5) Uani 1 1 d . . . O5 O 0.0767(3) 0.17843(15) 1.0137(2) 0.0337(6) Uani 1 1 d . . . O6 O 0.2868(3) 0.2375(2) 1.0022(3) 0.0568(9) Uani 1 1 d . . . N1 N 0.1597(5) 0.3346(2) 0.7293(4) 0.0523(10) Uani 1 1 d . . . C1 C 0.1696(3) -0.0443(2) 1.1446(3) 0.0219(6) Uani 1 1 d . . . C2 C 0.3133(3) 0.12329(19) 0.7663(3) 0.0212(6) Uani 1 1 d . . . C3 C 0.1718(4) 0.2348(2) 1.0411(3) 0.0295(8) Uani 1 1 d . . . C4 C 0.2861(3) -0.09330(18) 1.2202(3) 0.0196(6) Uani 1 1 d . . . C5 C 0.4269(3) -0.08377(19) 1.1982(3) 0.0194(6) Uani 1 1 d . . . C6 C 0.4639(3) 0.13127(18) 0.7386(3) 0.0188(6) Uani 1 1 d . . . C7 C 0.4963(3) 0.18917(19) 0.6525(3) 0.0211(6) Uani 1 1 d . . . C8 C 0.1360(3) 0.3009(2) 1.1293(3) 0.0222(7) Uani 1 1 d . . . C9 C 0.2548(3) -0.15034(19) 1.3072(3) 0.0222(7) Uani 1 1 d . . . C10 C 0.1023(6) 0.3572(3) 0.6006(5) 0.0641(14) Uani 1 1 d . . . H10A H 0.0846 0.4162 0.5953 0.096 Uiso 1 1 calc R . . H10B H 0.0146 0.3276 0.5756 0.096 Uiso 1 1 calc R . . H10C H 0.1707 0.3424 0.5480 0.096 Uiso 1 1 calc R . . C11 C 0.2993(6) 0.3733(3) 0.7705(5) 0.0678(15) Uani 1 1 d . . . H11A H 0.3667 0.3552 0.7188 0.102 Uiso 1 1 calc R . . H11B H 0.3324 0.3571 0.8536 0.102 Uiso 1 1 calc R . . H11C H 0.2901 0.4330 0.7661 0.102 Uiso 1 1 calc R . . O7 O 0.0182(4) 0.5925(2) 0.1256(4) 0.0718(10) Uiso 0.634(10) 1 d P A 1 N2 N 0.2458(5) 0.5900(3) 0.0853(5) 0.0718(13) Uiso 0.634(10) 1 d PD A 1 C12 C 0.1121(7) 0.5545(5) 0.0751(7) 0.050(2) Uiso 0.634(10) 1 d PD A 1 C13 C 0.2804(14) 0.6628(6) 0.1552(11) 0.099(4) Uiso 0.634(10) 1 d PD A 1 C14 C 0.3556(9) 0.5394(6) 0.0365(8) 0.062(2) Uiso 0.634(10) 1 d PD A 1 O7' O 0.0182(4) 0.5925(2) 0.1256(4) 0.0718(10) Uiso 0.366(10) 1 d P A 2 N2' N 0.2458(5) 0.5900(3) 0.0853(5) 0.0718(13) Uiso 0.366(10) 1 d PD A 2 C12' C 0.1355(15) 0.6351(10) 0.1373(14) 0.072(5) Uiso 0.366(10) 1 d PD A 2 C13' C 0.344(2) 0.6653(10) 0.101(2) 0.099(7) Uiso 0.366(10) 1 d PD A 2 C14' C 0.264(3) 0.5174(11) 0.015(2) 0.134(10) Uiso 0.366(10) 1 d PD A 2 H1 H 0.446(4) -0.047(2) 1.139(3) 0.023(9) Uiso 1 1 d . . . H2 H 0.415(4) 0.223(3) 0.604(4) 0.039(11) Uiso 1 1 d . . . H3 H 0.162(4) -0.158(2) 1.323(3) 0.019(8) Uiso 1 1 d . . . H4 H 0.089(4) 0.345(3) 0.775(4) 0.034(11) Uiso 1 1 d . . . H5 H 0.180(5) 0.270(3) 0.736(4) 0.053(13) Uiso 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 0.01227(18) 0.0190(2) 0.0229(2) -0.00027(14) 0.00679(13) 0.00080(13) O1 0.0231(12) 0.0502(16) 0.0355(15) 0.0221(12) 0.0106(11) 0.0107(11) O2 0.0137(10) 0.0378(13) 0.0264(12) -0.0042(10) 0.0061(9) -0.0007(9) O3 0.0191(10) 0.0196(11) 0.0338(13) 0.0029(9) 0.0144(10) 0.0014(8) O4 0.0183(10) 0.0288(12) 0.0382(14) 0.0043(11) 0.0067(10) 0.0053(9) O5 0.0309(13) 0.0283(13) 0.0448(16) -0.0176(11) 0.0148(11) -0.0029(10) O6 0.0380(15) 0.064(2) 0.076(2) -0.0424(18) 0.0333(15) -0.0116(14) N1 0.079(3) 0.0273(19) 0.052(2) 0.0070(17) 0.014(2) 0.0121(19) C1 0.0168(14) 0.0254(16) 0.0240(17) -0.0006(13) 0.0050(12) 0.0010(12) C2 0.0190(14) 0.0206(16) 0.0253(17) -0.0035(13) 0.0073(12) -0.0003(12) C3 0.0279(16) 0.0312(18) 0.0302(19) -0.0098(15) 0.0073(14) 0.0024(14) C4 0.0174(14) 0.0199(15) 0.0224(16) 0.0004(12) 0.0057(12) 0.0005(11) C5 0.0182(14) 0.0183(14) 0.0231(16) 0.0017(13) 0.0083(12) -0.0021(11) C6 0.0167(13) 0.0190(15) 0.0219(16) -0.0009(12) 0.0068(12) -0.0008(11) C7 0.0188(14) 0.0223(15) 0.0227(16) 0.0016(13) 0.0040(12) 0.0007(12) C8 0.0220(15) 0.0234(16) 0.0227(16) -0.0039(13) 0.0078(12) 0.0039(12) C9 0.0178(14) 0.0224(16) 0.0283(18) 0.0011(13) 0.0094(13) -0.0015(12) C10 0.086(4) 0.044(3) 0.058(3) 0.004(2) -0.006(3) 0.004(3) C11 0.096(4) 0.035(3) 0.067(3) -0.002(2) -0.006(3) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 1.927(2) . ? Zn1 O3 1.938(2) . ? Zn1 O2 1.964(2) . ? Zn1 O1 1.978(2) . ? O1 C1 1.248(4) . ? O2 C1 1.265(4) 3_557 ? O3 C2 1.273(4) . ? O4 C2 1.242(4) . ? O5 C3 1.278(4) . ? O6 C3 1.227(4) . ? N1 C11 1.469(7) . ? N1 C10 1.487(6) . ? N1 H4 0.91(4) . ? N1 H5 1.05(5) . ? C1 O2 1.265(4) 3_557 ? C1 C4 1.502(4) . ? C2 C6 1.505(4) . ? C3 C8 1.509(4) . ? C4 C9 1.388(4) . ? C4 C5 1.396(4) . ? C5 C6 1.385(4) 3_657 ? C5 H1 0.91(4) . ? C6 C5 1.385(4) 3_657 ? C6 C7 1.393(4) . ? C7 C8 1.391(4) 4_665 ? C7 H2 1.03(4) . ? C8 C7 1.391(4) 4_566 ? C8 C9 1.397(5) 2_557 ? C9 C8 1.397(4) 2_547 ? C9 H3 0.93(3) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? O7 C12 1.271(8) . ? N2 C12 1.374(7) . ? N2 C13 1.409(8) . ? N2 C14 1.479(7) . ? 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 O5 Zn1 O3 126.88(10) . . ? O5 Zn1 O2 103.57(10) . . ? O3 Zn1 O2 110.56(9) . . ? O5 Zn1 O1 108.90(12) . . ? O3 Zn1 O1 93.07(9) . . ? O2 Zn1 O1 113.96(11) . . ? C1 O1 Zn1 142.3(2) . . ? C1 O2 Zn1 126.4(2) 3_557 . ? C2 O3 Zn1 117.87(19) . . ? C3 O5 Zn1 117.5(2) . . ? C11 N1 C10 112.2(4) . . ? C11 N1 H4 117(3) . . ? C10 N1 H4 107(3) . . ? C11 N1 H5 104(2) . . ? C10 N1 H5 110(3) . . ? H4 N1 H5 106(4) . . ? O1 C1 O2 125.4(3) . 3_557 ? O1 C1 C4 116.8(3) . . ? O2 C1 C4 117.8(3) 3_557 . ? O4 C2 O3 124.4(3) . . ? O4 C2 C6 120.1(3) . . ? O3 C2 C6 115.5(3) . . ? O6 C3 O5 124.8(3) . . ? O6 C3 C8 119.7(3) . . ? O5 C3 C8 115.5(3) . . ? C9 C4 C5 119.9(3) . . ? C9 C4 C1 120.9(3) . . ? C5 C4 C1 119.2(3) . . ? C6 C5 C4 120.8(3) 3_657 . ? C6 C5 H1 120(2) 3_657 . ? C4 C5 H1 119(2) . . ? C5 C6 C7 119.1(3) 3_657 . ? C5 C6 C2 120.5(3) 3_657 . ? C7 C6 C2 120.3(3) . . ? C8 C7 C6 120.8(3) 4_665 . ? C8 C7 H2 120(2) 4_665 . ? C6 C7 H2 119(2) . . ? C7 C8 C9 119.7(3) 4_566 2_557 ? C7 C8 C3 120.5(3) 4_566 . ? C9 C8 C3 119.7(3) 2_557 . ? C4 C9 C8 119.8(3) . 2_547 ? C4 C9 H3 122(2) . . ? C8 C9 H3 118(2) 2_547 . ? 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 . . ? C12 N2 C13 121.5(7) . . ? C12 N2 C14 115.5(6) . . ? C13 N2 C14 122.2(7) . . ? O7 C12 N2 117.4(6) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.286 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.105