Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_p4n _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Yang, Shi-Yao' ; School of Chemistry and Chemical Engineering Xiamen University Xiamen 361005 P. R. China ; 'Long, La-Sheng' ; School of Chemistry and Chemical Engineering Xiamen University Xiamen 361005 P. R. China ; 'Huang, Rong-Bin' ; School of Chemistry and Chemical Engineering Xiamen University Xiamen 361005 P. R. China ; 'Zheng, Lan-Sun' ; School of Chemistry and Chemical Engineering Xiamen University Xiamen 361005 P. R. China ; _publ_contact_author_name 'Dr La-Sheng Long' _publ_contact_author_address ; Department of chemistry xiamen university Department of chemistry,xiamen univ xiamen china 361005 CHINA ; _publ_contact_author_email 'LSLONG@JINGXIAN.XMU.EDU.CN' _publ_section_title ; [Zn8(SiO4)(C8H4O4)6]n: Firstborn of a New Metal Silicate - Organic Hybrid Material Family (C8H4O4 = isophthalate) ; _database_code_CSD 167834 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H28 O30 Si Zn8' _chemical_formula_weight 1635.75 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' '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' 'Si' 'Si' 0.0817 0.0704 '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 Tetragonal _symmetry_space_group_name_H-M P4(2)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 13.7409(19) _cell_length_b 13.7409(19) _cell_length_c 14.976(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2827.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 15 _exptl_crystal_description octahedron _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.921 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1620 _exptl_absorpt_coefficient_mu 3.447 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.91868 _exptl_absorpt_correction_T_max 0.99852 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Enraf Nonius CAD4' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% none _diffrn_reflns_number 3008 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -2 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.98 _reflns_number_total 2764 _reflns_number_gt 1891 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _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. ; _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^)+(0.0478P)^2^+2.2708P] 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 2764 _refine_ls_number_parameters 202 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1194 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.007 _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 0.11914(5) 0.11553(5) 0.37818(5) 0.0306(2) Uani 1 1 d . . . Zn2 Zn 0.04150(5) 0.31659(5) 0.32479(4) 0.0274(2) Uani 1 1 d . . . O1 O 0.0729(4) 0.1576(3) 0.4934(3) 0.0474(13) Uani 1 1 d . . . Si1 Si 0.2500 0.2500 0.2500 0.0216(7) Uani 1 4 d S . . O2 O 0.0082(3) 0.2988(3) 0.4507(3) 0.0429(12) Uani 1 1 d . . . O3 O -0.0578(3) 0.5433(3) 0.6788(3) 0.0392(11) Uani 1 1 d . . . O4 O -0.0680(3) 0.4994(3) 0.8228(3) 0.0421(12) Uani 1 1 d . . . O5 O 0.2013(4) 0.0038(3) 0.3823(3) 0.0513(14) Uani 1 1 d . . . O6 O 0.2127(3) -0.0712(3) 0.2515(3) 0.0428(12) Uani 1 1 d . . . O7 O 0.1533(3) 0.2312(3) 0.3098(3) 0.0278(9) Uani 1 1 d . . . C1 C 0.0315(5) 0.2372(5) 0.5087(4) 0.0359(15) Uani 1 1 d . . . C2 C -0.0144(4) 0.3561(4) 0.6268(4) 0.0302(14) Uani 1 1 d . . . H2 H -0.0211 0.4036 0.5830 0.036 Uiso 1 1 calc R . . C3 C 0.0109(5) 0.2618(5) 0.6030(4) 0.0327(15) Uani 1 1 d . . . C4 C 0.0201(6) 0.1913(5) 0.6692(4) 0.0459(19) Uani 1 1 d . . . H4 H 0.0379 0.1282 0.6540 0.055 Uiso 1 1 calc R . . C5 C 0.0027(6) 0.2152(5) 0.7579(5) 0.052(2) Uani 1 1 d . . . H5 H 0.0075 0.1677 0.8019 0.062 Uiso 1 1 calc R . . C6 C -0.0216(5) 0.3089(5) 0.7805(4) 0.0406(17) Uani 1 1 d . . . H6 H -0.0325 0.3249 0.8400 0.049 Uiso 1 1 calc R . . C7 C -0.0298(5) 0.3794(4) 0.7155(4) 0.0296(14) Uani 1 1 d . . . C8 C -0.0551(4) 0.4821(5) 0.7418(4) 0.0308(14) Uani 1 1 d . . . C9 C 0.2141(5) -0.0710(5) 0.3348(5) 0.0362(15) Uani 1 1 d . . . C10 C 0.2500 -0.2500 0.3354(6) 0.033(2) Uani 1 2 d S . . H10 H 0.2500 -0.2500 0.2733 0.040 Uiso 1 2 calc SR . . C11 C 0.2333(5) -0.1636(5) 0.3827(4) 0.0346(15) Uani 1 1 d . . . C12 C 0.2332(6) -0.1650(6) 0.4752(5) 0.060(2) Uani 1 1 d . . . H12 H 0.2216 -0.1080 0.5070 0.072 Uiso 1 1 calc R . . C13 C 0.2500 -0.2500 0.5195(7) 0.076(4) Uani 1 2 d S . . H13 H 0.2500 -0.2500 0.5816 0.091 Uiso 1 2 calc SR . . O1W O 0.261(2) 0.137(2) 0.4781(19) 0.103(9) Uiso 0.25 1 d P . . H1WA H 0.2470 0.0797 0.4950 0.154 Uiso 0.25 1 d PR . . H1WB H 0.2995 0.1328 0.4342 0.154 Uiso 0.25 1 d PR . . O2W O 0.2500 0.2500 0.620(3) 0.27(2) Uani 0.50 2 d SP . . H2WA H 0.1935 0.2301 0.6057 0.400 Uiso 0.25 1 d PR . . H2WB H 0.2825 0.2572 0.5722 0.400 Uiso 0.25 1 d PR . . 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 0.0389(5) 0.0228(4) 0.0301(4) -0.0009(3) 0.0058(3) 0.0015(3) Zn2 0.0278(4) 0.0307(4) 0.0236(4) 0.0018(3) 0.0011(3) 0.0062(3) O1 0.081(4) 0.033(3) 0.028(2) -0.002(2) 0.008(2) 0.013(3) Si1 0.0196(10) 0.0196(10) 0.0257(17) 0.000 0.000 0.000 O2 0.052(3) 0.053(3) 0.024(2) 0.006(2) 0.011(2) 0.013(2) O3 0.056(3) 0.026(2) 0.035(3) 0.001(2) -0.001(2) 0.008(2) O4 0.055(3) 0.043(3) 0.029(2) -0.006(2) 0.001(2) 0.011(2) O5 0.063(3) 0.032(3) 0.059(3) -0.006(3) -0.006(3) 0.017(2) O6 0.051(3) 0.032(3) 0.045(3) 0.012(2) -0.002(2) 0.001(2) O7 0.029(2) 0.022(2) 0.032(2) 0.0037(18) 0.0046(19) 0.0014(17) C1 0.041(4) 0.034(4) 0.033(4) -0.002(3) -0.002(3) -0.002(3) C2 0.036(4) 0.029(3) 0.026(3) 0.005(3) 0.005(3) 0.000(3) C3 0.043(4) 0.030(3) 0.025(3) -0.001(3) 0.004(3) 0.003(3) C4 0.086(6) 0.026(4) 0.027(3) 0.005(3) 0.003(4) 0.011(4) C5 0.094(6) 0.033(4) 0.029(4) 0.015(3) 0.009(4) 0.006(4) C6 0.064(5) 0.031(4) 0.026(3) 0.002(3) 0.004(3) 0.000(3) C7 0.035(4) 0.029(3) 0.025(3) 0.000(3) 0.003(3) 0.003(3) C8 0.028(3) 0.035(4) 0.030(4) 0.002(3) 0.001(3) -0.002(3) C9 0.027(3) 0.038(4) 0.043(4) 0.001(3) 0.000(3) 0.002(3) C10 0.030(5) 0.039(5) 0.031(5) 0.000 0.000 0.007(4) C11 0.036(4) 0.033(4) 0.035(4) 0.000(3) 0.007(3) 0.006(3) C12 0.099(7) 0.044(5) 0.037(4) -0.012(4) 0.009(4) 0.018(4) C13 0.149(13) 0.049(7) 0.028(6) 0.000 0.000 0.024(8) O2W 0.15(3) 0.41(7) 0.24(4) 0.000 0.000 -0.10(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 O5 1.906(5) . ? Zn1 O1 1.927(4) . ? Zn1 O7 1.948(4) . ? Zn1 O4 1.956(4) 4_454 ? Zn1 O1W 2.47(3) . ? Zn1 Zn2 3.0676(11) . ? Zn2 O3 1.938(4) 5_566 ? Zn2 O7 1.946(4) . ? Zn2 O2 1.956(4) . ? Zn2 O6 1.966(4) 7_566 ? O1 C1 1.254(8) . ? Si1 O7 1.623(4) 2 ? Si1 O7 1.623(4) 7_566 ? Si1 O7 1.623(4) 8_656 ? Si1 O7 1.623(4) . ? O2 C1 1.254(7) . ? O3 C8 1.265(7) . ? O3 Zn2 1.938(4) 5_566 ? O4 C8 1.249(7) . ? O4 Zn1 1.956(4) 3 ? O5 C9 1.263(8) . ? O6 C9 1.248(7) . ? O6 Zn2 1.966(4) 8_656 ? C1 C3 1.480(9) . ? C2 C7 1.383(8) . ? C2 C3 1.388(8) . ? C3 C4 1.391(8) . ? C4 C5 1.389(9) . ? C5 C6 1.373(9) . ? C6 C7 1.378(8) . ? C7 C8 1.505(8) . ? C9 C11 1.485(9) . ? C10 C11 1.401(8) 2_545 ? C10 C11 1.401(8) . ? C11 C12 1.385(9) . ? C12 C13 1.363(9) . ? C13 C12 1.363(9) 2_545 ? 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 O1 114.1(2) . . ? O5 Zn1 O7 122.1(2) . . ? O1 Zn1 O7 107.79(18) . . ? O5 Zn1 O4 104.1(2) . 4_454 ? O1 Zn1 O4 101.7(2) . 4_454 ? O7 Zn1 O4 104.59(18) . 4_454 ? O5 Zn1 O1W 67.1(7) . . ? O1 Zn1 O1W 71.4(7) . . ? O7 Zn1 O1W 91.8(7) . . ? O4 Zn1 O1W 163.6(7) 4_454 . ? O5 Zn1 Zn2 159.98(17) . . ? O1 Zn1 Zn2 81.29(14) . . ? O7 Zn1 Zn2 38.00(11) . . ? O4 Zn1 Zn2 84.10(14) 4_454 . ? O1W Zn1 Zn2 108.9(7) . . ? O3 Zn2 O7 120.31(18) 5_566 . ? O3 Zn2 O2 100.2(2) 5_566 . ? O7 Zn2 O2 102.75(18) . . ? O3 Zn2 O6 106.13(19) 5_566 7_566 ? O7 Zn2 O6 115.53(18) . 7_566 ? O2 Zn2 O6 110.5(2) . 7_566 ? O3 Zn2 Zn1 149.48(14) 5_566 . ? O7 Zn2 Zn1 38.04(11) . . ? O2 Zn2 Zn1 73.61(14) . . ? O6 Zn2 Zn1 103.94(14) 7_566 . ? C1 O1 Zn1 125.1(4) . . ? O7 Si1 O7 107.72(14) 2 7_566 ? O7 Si1 O7 107.72(13) 2 8_656 ? O7 Si1 O7 113.0(3) 7_566 8_656 ? O7 Si1 O7 113.0(3) 2 . ? O7 Si1 O7 107.72(13) 7_566 . ? O7 Si1 O7 107.72(14) 8_656 . ? C1 O2 Zn2 133.8(4) . . ? C8 O3 Zn2 132.7(4) . 5_566 ? C8 O4 Zn1 128.3(4) . 3 ? C9 O5 Zn1 136.0(5) . . ? C9 O6 Zn2 125.6(5) . 8_656 ? Si1 O7 Zn2 127.9(2) . . ? Si1 O7 Zn1 128.1(2) . . ? Zn2 O7 Zn1 103.96(18) . . ? O2 C1 O1 125.3(6) . . ? O2 C1 C3 117.2(6) . . ? O1 C1 C3 117.4(6) . . ? C7 C2 C3 120.0(6) . . ? C2 C3 C4 119.3(6) . . ? C2 C3 C1 120.4(6) . . ? C4 C3 C1 120.2(6) . . ? C5 C4 C3 120.1(6) . . ? C6 C5 C4 120.0(6) . . ? C5 C6 C7 120.3(6) . . ? C6 C7 C2 120.2(6) . . ? C6 C7 C8 119.6(6) . . ? C2 C7 C8 120.2(5) . . ? O4 C8 O3 126.4(6) . . ? O4 C8 C7 117.7(6) . . ? O3 C8 C7 115.9(5) . . ? O6 C9 O5 124.3(7) . . ? O6 C9 C11 118.9(6) . . ? O5 C9 C11 116.8(6) . . ? C11 C10 C11 119.2(9) 2_545 . ? C12 C11 C10 119.6(7) . . ? C12 C11 C9 119.6(6) . . ? C10 C11 C9 120.7(6) . . ? C13 C12 C11 119.9(8) . . ? C12 C13 C12 121.7(10) 2_545 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.713 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.109