# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Feng Luo' _publ_contact_author_email ECIT.LUOFENG@GMAIL.COM _publ_section_title ; Metal-organic framework (MOF): lanthanide(III)-doped approach for luminescence modulation and luminescent sensing ; loop_ _publ_author_name 'Feng Luo.' 'Stuart R. Batten' # Attachment '1-R.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 721176' #TrackingRef '1-R.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10 N2 O8 Zn' _chemical_formula_weight 351.60 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' 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' N N 0.0061 0.0033 '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 11.548(2) _cell_length_b 15.319(3) _cell_length_c 11.021(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.36(3) _cell_angle_gamma 90.00 _cell_volume 1947.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7216 _cell_measurement_theta_min 3.24 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 1.289 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7826 _exptl_absorpt_correction_T_max 0.8504 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9467 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2232 _reflns_number_gt 1906 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The platon Squeeze program is used to treat the badly disordered water molecules. ; _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^)+(0.0693P)^2^+0.2729P] 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 2232 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.1105 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 C1 C 0.8051(2) 0.30559(15) 0.4197(2) 0.0272(5) Uani 1 1 d . . . C2 C 0.8595(2) 0.36456(17) 0.3290(2) 0.0325(6) Uani 1 1 d . . . C3 C 0.8323(2) 0.31049(15) 0.5440(2) 0.0263(5) Uani 1 1 d . . . C4 C 0.7770(2) 0.25511(16) 0.6221(2) 0.0299(5) Uani 1 1 d . . . H4 H 0.7952 0.2585 0.7050 0.036 Uiso 1 1 calc R . . C5 C 0.9220(2) 0.37056(16) 0.6000(2) 0.0277(5) Uani 1 1 d . . . N1 N 0.2261(3) 0.4246(2) 0.5050(3) 0.0636(8) Uani 1 1 d . . . O1 O 0.90931(16) 0.43252(11) 0.37085(16) 0.0339(4) Uani 1 1 d . . . O2 O 0.8524(2) 0.34606(16) 0.22005(19) 0.0613(7) Uani 1 1 d . . . O3 O 1.02589(16) 0.34842(13) 0.60042(19) 0.0415(5) Uani 1 1 d . . . O4 O 0.88438(15) 0.43822(11) 0.65131(16) 0.0311(4) Uani 1 1 d . . . Zn1 Zn 1.0000 0.49461(2) 0.2500 0.02181(15) 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 C1 0.0362(13) 0.0240(11) 0.0216(12) 0.0009(9) 0.0033(9) -0.0056(10) C2 0.0404(15) 0.0315(13) 0.0257(13) 0.0035(10) 0.0023(10) -0.0077(11) C3 0.0355(13) 0.0196(11) 0.0238(12) 0.0000(9) 0.0021(9) -0.0050(9) C4 0.0416(14) 0.0287(12) 0.0193(11) 0.0005(9) 0.0000(9) -0.0085(10) C5 0.0344(14) 0.0277(12) 0.0212(12) 0.0013(9) 0.0016(9) -0.0096(10) N1 0.0631(19) 0.0654(19) 0.063(2) 0.0010(15) 0.0063(15) 0.0112(15) O1 0.0474(11) 0.0270(9) 0.0279(10) 0.0032(7) 0.0101(7) -0.0130(8) O2 0.0952(18) 0.0659(15) 0.0230(11) -0.0006(10) 0.0060(10) -0.0437(13) O3 0.0350(11) 0.0441(11) 0.0453(12) -0.0093(9) -0.0003(8) -0.0038(9) O4 0.0374(10) 0.0267(9) 0.0292(9) -0.0038(7) 0.0004(7) -0.0064(7) Zn1 0.0287(3) 0.0190(2) 0.0179(2) 0.000 0.00328(15) 0.000 _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 C4 1.393(3) 7_656 ? C1 C3 1.395(3) . ? C1 C2 1.504(3) . ? C2 O2 1.234(3) . ? C2 O1 1.267(3) . ? C3 C4 1.383(3) . ? C3 C5 1.499(3) . ? C4 C1 1.393(3) 7_656 ? C4 H4 0.9300 . ? C5 O3 1.247(3) . ? C5 O4 1.266(3) . ? O1 Zn1 1.9724(17) . ? O4 Zn1 1.9761(17) 5_766 ? Zn1 O1 1.9724(17) 2_755 ? Zn1 O4 1.9761(17) 5_766 ? Zn1 O4 1.9761(17) 6_565 ? 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 C4 C1 C3 118.9(2) 7_656 . ? C4 C1 C2 118.6(2) 7_656 . ? C3 C1 C2 122.5(2) . . ? O2 C2 O1 123.6(2) . . ? O2 C2 C1 119.8(2) . . ? O1 C2 C1 116.6(2) . . ? C4 C3 C1 119.1(2) . . ? C4 C3 C5 116.7(2) . . ? C1 C3 C5 124.1(2) . . ? C3 C4 C1 121.9(2) . 7_656 ? C3 C4 H4 119.0 . . ? C1 C4 H4 119.0 7_656 . ? O3 C5 O4 124.7(2) . . ? O3 C5 C3 118.9(2) . . ? O4 C5 C3 116.3(2) . . ? C2 O1 Zn1 113.36(17) . . ? C5 O4 Zn1 115.83(16) . 5_766 ? O1 Zn1 O1 122.34(11) 2_755 . ? O1 Zn1 O4 104.91(8) 2_755 5_766 ? O1 Zn1 O4 104.18(7) . 5_766 ? O1 Zn1 O4 104.18(7) 2_755 6_565 ? O1 Zn1 O4 104.91(8) . 6_565 ? O4 Zn1 O4 117.24(10) 5_766 6_565 ? 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 C4 C1 C2 O2 -16.8(4) 7_656 . . . ? C3 C1 C2 O2 164.4(3) . . . . ? C4 C1 C2 O1 162.1(2) 7_656 . . . ? C3 C1 C2 O1 -16.7(4) . . . . ? C4 C1 C3 C4 -0.1(4) 7_656 . . . ? C2 C1 C3 C4 178.8(2) . . . . ? C4 C1 C3 C5 177.7(2) 7_656 . . . ? C2 C1 C3 C5 -3.5(4) . . . . ? C1 C3 C4 C1 0.1(4) . . . 7_656 ? C5 C3 C4 C1 -177.9(2) . . . 7_656 ? C4 C3 C5 O3 96.1(3) . . . . ? C1 C3 C5 O3 -81.8(3) . . . . ? C4 C3 C5 O4 -79.2(3) . . . . ? C1 C3 C5 O4 103.0(3) . . . . ? O2 C2 O1 Zn1 -10.9(4) . . . . ? C1 C2 O1 Zn1 170.20(17) . . . . ? O3 C5 O4 Zn1 -5.7(3) . . . 5_766 ? C3 C5 O4 Zn1 169.24(16) . . . 5_766 ? C2 O1 Zn1 O1 -38.38(16) . . . 2_755 ? C2 O1 Zn1 O4 -156.68(18) . . . 5_766 ? C2 O1 Zn1 O4 79.56(19) . . . 6_565 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.418 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.083 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 0.000 0.000 -0.011 422 65 ' ' 2 0.500 0.500 -0.013 421 65 ' ' _platon_squeeze_details ; ;