# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 1145/189 data_UiO-17 _publ_contact_author_name ; Helmer Fjellvg University of Oslo P.O Box 1033 Blindern N-0315 Oslo Norway ; _publ_requested_journal 'Journal of Materials Chemistry' _publ_section_title ; The synthesis and crystal structure of a new open-framework zincophosphate UiO-17 ; _audit_creation_method 'SHELXL-97' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H28 N4 O26 P6 Zn7' _chemical_formula_weight 1239.75 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' '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' 'P' 'P' 0.1023 0.0942 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.134(3) _cell_length_b 8.2407(16) _cell_length_c 22.860(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.05(3) _cell_angle_gamma 90.00 _cell_volume 2948.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 23.35 _exptl_crystal_description 'rectangular' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 6.039 _exptl_absorpt_correction_type 'Empirical with SADABS' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Siemens SMART CCD' _diffrn_measurement_method 'scanning' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30302 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 40.32 _reflns_number_total 8890 _reflns_number_gt 8039 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART CCD' _computing_cell_refinement 'SMART' _computing_data_reduction 'SAINT' _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^)+(0.0467P)^2^+10.7537P] 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 SHELXL _refine_ls_extinction_coef 0.00271(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8890 _refine_ls_number_parameters 233 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0909 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.198467(12) 0.15525(2) 0.073721(9) 0.00472(4) Uani 1 1 d . . . Zn2 Zn -0.148858(12) 0.35073(2) 0.072540(9) 0.00473(4) Uani 1 1 d . . . Zn3 Zn 0.236331(13) 0.38359(2) 0.194069(9) 0.00577(4) Uani 1 1 d . . . Zn4 Zn 0.0000 0.32850(3) 0.2500 0.00508(5) Uani 1 2 d S . . P1 P 0.26823(3) 0.48935(5) 0.045514(19) 0.00429(7) Uani 1 1 d . . . P2 P 0.05122(3) 0.28965(5) 0.132536(19) 0.00425(7) Uani 1 1 d . . . P3 P 0.18066(3) 0.51044(5) 0.310495(19) 0.00396(7) Uani 1 1 d . . . O1 O -0.18239(9) 0.46270(18) -0.00405(6) 0.0101(2) Uani 1 1 d . . . O2 O -0.18683(10) 0.13400(16) 0.08294(6) 0.0099(2) Uani 1 1 d . . . O3 O 0.25521(9) 0.36258(15) 0.09229(6) 0.00795(19) Uani 1 1 d . . . O4 O 0.17178(9) 0.08419(18) -0.00901(6) 0.0096(2) Uani 1 1 d . . . O5 O 0.09014(8) 0.15924(16) 0.09760(6) 0.00717(19) Uani 1 1 d . . . O6 O 0.02394(9) 0.20143(16) 0.18413(6) 0.0084(2) Uani 1 1 d . . . O7 O -0.02558(8) 0.37357(16) 0.08915(6) 0.00713(19) Uani 1 1 d . . . O8 O 0.11781(8) 0.42190(16) 0.15665(6) 0.00744(19) Uani 1 1 d . . . O9 O 0.28581(8) -0.00547(15) 0.11875(6) 0.00640(18) Uani 1 1 d . . . O10 O 0.29560(9) 0.17809(16) 0.20799(6) 0.0095(2) Uani 1 1 d . . . O11 O 0.08494(8) 0.48315(17) 0.29500(6) 0.0090(2) Uani 1 1 d . . . O12 O 0.22733(8) 0.37885(16) 0.28220(6) 0.00719(19) Uani 1 1 d . . . OW O 0.31823(9) 0.56683(17) 0.19885(6) 0.0099(2) Uani 1 1 d . . . N1 N 0.10984(10) 0.85660(19) 0.14947(8) 0.0092(2) Uani 1 1 d . . . H1A H 0.1624 0.8475 0.1742 0.018(3) Uiso 1 1 calc R . . H1B H 0.1008 0.9621 0.1398 0.018(3) Uiso 1 1 calc R . . N2 N -0.04686(11) 0.7170(2) 0.08434(8) 0.0119(3) Uani 1 1 d . . . H2A H -0.0995 0.7255 0.0597 0.018(3) Uiso 1 1 calc R . . H2B H -0.0377 0.6118 0.0946 0.018(3) Uiso 1 1 calc R . . C1 C -0.04254(11) 0.8153(2) 0.13990(9) 0.0106(3) Uani 1 1 d . . . H1A H -0.0853 0.7773 0.1601 0.018(3) Uiso 1 1 calc R . . H1B H -0.0545 0.9282 0.1290 0.018(3) Uiso 1 1 calc R . . C2 C 0.04528(12) 0.8009(2) 0.18199(8) 0.0104(3) Uani 1 1 d . . . H2A H 0.0486 0.8671 0.2176 0.018(3) Uiso 1 1 calc R . . H2B H 0.0564 0.6890 0.1947 0.018(3) Uiso 1 1 calc R . . C3 C 0.10648(12) 0.7613(2) 0.09332(9) 0.0107(3) Uani 1 1 d . . . H3A H 0.1203 0.6487 0.1036 0.018(3) Uiso 1 1 calc R . . H3B H 0.1484 0.8034 0.0732 0.018(3) Uiso 1 1 calc R . . C4 C 0.01825(13) 0.7724(2) 0.05154(9) 0.0128(3) Uani 1 1 d . . . H4A H 0.0065 0.8836 0.0381 0.018(3) Uiso 1 1 calc R . . H4B H 0.0152 0.7048 0.0164 0.018(3) 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 0.00532(8) 0.00295(8) 0.00617(8) -0.00026(5) 0.00191(6) 0.00001(5) Zn2 0.00445(7) 0.00263(7) 0.00702(8) 0.00049(5) 0.00123(6) -0.00010(5) Zn3 0.00513(7) 0.00340(8) 0.00826(8) -0.00030(5) 0.00063(6) 0.00050(5) Zn4 0.00495(10) 0.00442(10) 0.00584(10) 0.000 0.00123(8) 0.000 P1 0.00534(15) 0.00227(14) 0.00528(15) 0.00022(11) 0.00133(12) 0.00028(12) P2 0.00401(14) 0.00291(15) 0.00585(15) -0.00013(11) 0.00127(12) 0.00039(11) P3 0.00428(14) 0.00226(14) 0.00531(15) -0.00030(11) 0.00114(12) -0.00067(11) O1 0.0082(5) 0.0135(6) 0.0083(5) 0.0045(4) 0.0014(4) 0.0036(4) O2 0.0163(6) 0.0041(5) 0.0099(5) -0.0015(4) 0.0041(4) -0.0042(4) O3 0.0108(5) 0.0037(4) 0.0085(5) 0.0018(3) 0.0008(4) -0.0025(4) O4 0.0083(5) 0.0127(6) 0.0078(5) -0.0032(4) 0.0021(4) 0.0039(4) O5 0.0068(4) 0.0053(5) 0.0104(5) -0.0016(3) 0.0041(4) 0.0005(4) O6 0.0124(5) 0.0057(5) 0.0083(5) 0.0011(3) 0.0050(4) 0.0007(4) O7 0.0048(4) 0.0070(5) 0.0088(5) 0.0014(3) 0.0001(4) 0.0012(4) O8 0.0052(4) 0.0047(5) 0.0109(5) -0.0015(4) -0.0008(4) -0.0006(4) O9 0.0088(5) 0.0053(4) 0.0050(4) 0.0003(3) 0.0014(4) 0.0024(4) O10 0.0147(6) 0.0048(5) 0.0092(5) -0.0003(4) 0.0029(4) 0.0041(4) O11 0.0050(4) 0.0098(5) 0.0119(5) -0.0034(4) 0.0019(4) -0.0021(4) O12 0.0084(5) 0.0057(5) 0.0076(5) -0.0009(3) 0.0020(4) 0.0026(4) OW 0.0134(5) 0.0064(5) 0.0105(5) -0.0015(4) 0.0042(4) -0.0034(4) N1 0.0067(5) 0.0063(5) 0.0140(6) 0.0001(4) 0.0011(5) -0.0008(4) N2 0.0081(6) 0.0084(6) 0.0166(7) 0.0001(5) -0.0022(5) -0.0010(5) C1 0.0069(6) 0.0083(6) 0.0161(7) 0.0022(5) 0.0020(5) -0.0008(5) C2 0.0102(6) 0.0102(7) 0.0108(6) 0.0021(5) 0.0023(5) -0.0005(5) C3 0.0110(6) 0.0077(6) 0.0144(7) 0.0001(5) 0.0049(5) 0.0003(5) C4 0.0145(7) 0.0126(7) 0.0103(7) 0.0002(5) 0.0009(6) 0.0007(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 1.9260(14) . ? Zn1 O3 1.9361(13) . ? Zn1 O5 1.9537(13) . ? Zn1 O9 2.0237(13) . ? Zn2 O2 1.9216(14) . ? Zn2 O1 1.9363(14) . ? Zn2 O7 1.9412(13) . ? Zn2 O9 2.0424(13) 3_455 ? Zn3 O8 1.9218(14) . ? Zn3 O10 1.9328(14) . ? Zn3 OW 1.9919(14) . ? Zn3 O12 2.0551(14) . ? Zn3 O3 2.4250(15) . ? Zn4 O6 1.9480(14) 2 ? Zn4 O6 1.9481(14) . ? Zn4 O11 1.9687(14) . ? Zn4 O11 1.9688(14) 2 ? P1 O1 1.5282(15) 5_565 ? P1 O2 1.5418(14) 3 ? P1 O3 1.5453(13) . ? P1 O4 1.5469(14) 7 ? P2 O8 1.5356(14) . ? P2 O6 1.5381(14) . ? P2 O7 1.5494(14) . ? P2 O5 1.5590(13) . ? P3 O11 1.5149(14) . ? P3 O10 1.5208(14) 4 ? P3 O12 1.5485(13) . ? P3 O9 1.5814(14) 4 ? O1 P1 1.5283(15) 5_565 ? O2 P1 1.5418(14) 3_445 ? O4 P1 1.5469(14) 7 ? O9 P3 1.5815(14) 4_545 ? O9 Zn2 2.0425(13) 3_545 ? O10 P3 1.5208(14) 4_545 ? N1 C2 1.491(2) . ? N1 C3 1.494(3) . ? N2 C1 1.494(3) . ? N2 C4 1.502(3) . ? C1 C2 1.512(3) . ? C3 C4 1.512(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O3 117.69(6) . . ? O4 Zn1 O5 106.12(6) . . ? O3 Zn1 O5 109.35(6) . . ? O4 Zn1 O9 105.22(6) . . ? O3 Zn1 O9 103.43(6) . . ? O5 Zn1 O9 115.38(6) . . ? O2 Zn2 O1 121.82(7) . . ? O2 Zn2 O7 114.09(6) . . ? O1 Zn2 O7 100.30(6) . . ? O2 Zn2 O9 104.79(6) . 3_455 ? O1 Zn2 O9 97.19(6) . 3_455 ? O7 Zn2 O9 118.39(6) . 3_455 ? O8 Zn3 O10 128.04(6) . . ? O8 Zn3 OW 118.36(6) . . ? O10 Zn3 OW 111.11(7) . . ? O8 Zn3 O12 98.05(6) . . ? O10 Zn3 O12 88.38(6) . . ? OW Zn3 O12 99.47(6) . . ? O8 Zn3 O3 85.86(6) . . ? O10 Zn3 O3 85.59(5) . . ? OW Zn3 O3 82.56(5) . . ? O12 Zn3 O3 173.97(5) . . ? O6 Zn4 O6 114.97(8) 2 . ? O6 Zn4 O11 100.81(6) 2 . ? O6 Zn4 O11 120.55(6) . . ? O6 Zn4 O11 120.56(6) 2 2 ? O6 Zn4 O11 100.81(6) . 2 ? O11 Zn4 O11 99.32(9) . 2 ? O1 P1 O2 112.18(9) 5_565 3 ? O1 P1 O3 110.43(8) 5_565 . ? O2 P1 O3 105.27(8) 3 . ? O1 P1 O4 110.98(8) 5_565 7 ? O2 P1 O4 109.32(8) 3 7 ? O3 P1 O4 108.45(8) . 7 ? O8 P2 O6 111.45(8) . . ? O8 P2 O7 107.11(8) . . ? O6 P2 O7 111.62(8) . . ? O8 P2 O5 109.84(7) . . ? O6 P2 O5 107.03(8) . . ? O7 P2 O5 109.80(8) . . ? O11 P3 O10 112.40(8) . 4 ? O11 P3 O12 111.70(8) . . ? O10 P3 O12 109.83(8) 4 . ? O11 P3 O9 107.64(8) . 4 ? O10 P3 O9 108.23(7) 4 4 ? O12 P3 O9 106.79(7) . 4 ? P1 O1 Zn2 134.13(9) 5_565 . ? P1 O2 Zn2 140.45(9) 3_445 . ? P1 O3 Zn1 125.55(8) . . ? P1 O3 Zn3 133.27(8) . . ? Zn1 O3 Zn3 96.35(5) . . ? P1 O4 Zn1 128.98(9) 7 . ? P2 O5 Zn1 130.81(8) . . ? P2 O6 Zn4 119.08(8) . . ? P2 O7 Zn2 134.76(8) . . ? P2 O8 Zn3 125.24(8) . . ? P3 O9 Zn1 119.28(7) 4_545 . ? P3 O9 Zn2 119.06(7) 4_545 3_545 ? Zn1 O9 Zn2 119.98(6) . 3_545 ? P3 O10 Zn3 153.92(9) 4_545 . ? P3 O11 Zn4 139.38(9) . . ? P3 O12 Zn3 123.61(8) . . ? C2 N1 C3 112.48(14) . . ? C1 N2 C4 111.42(15) . . ? N2 C1 C2 109.96(15) . . ? N1 C2 C1 108.58(15) . . ? N1 C3 C4 110.07(15) . . ? N2 C4 C3 109.35(16) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 40.32 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 1.931 _refine_diff_density_min -1.166 _refine_diff_density_rms 0.185 #==END