# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Enbo Wang' _publ_contact_author_address ; Department of Chemistry Northeast Normal University Institute of Polyoxometalate Chemis Changchun 130024 CHINA ; _publ_contact_author_email WANGENBO@PUBLIC.CC.JL.CN _publ_section_title ; >From arm-shaped layers to a new type of polythreaded array: a two fold interpenetrated three-dimensional network with the rutile topology ; loop_ _publ_author_name 'Enbo Wang' 'Lucia Carlucci' 'Changwen Hu' 'Chao Qin' 'Ming-Liang Tong' 'Xinlong Wang' 'Lin Xu' data_zn _database_code_depnum_ccdc_archive 'CCDC 233352' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H12 N2 O6 Zn' _chemical_formula_weight 429.68 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 9.869(2) _cell_length_b 16.781(3) _cell_length_c 11.299(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.02(3) _cell_angle_gamma 90.00 _cell_volume 1842.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 7284 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.48 _exptl_crystal_description colorless _exptl_crystal_colour block _exptl_crystal_size_max 0.362 _exptl_crystal_size_mid 0.337 _exptl_crystal_size_min 0.241 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 1.372 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.615 _exptl_absorpt_correction_T_max 0.718 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_decay_% ? _diffrn_reflns_number 7284 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4122 _reflns_number_gt 2484 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _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^)+(0.0920P)^2^+1.6347P] 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 0.0034(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4122 _refine_ls_number_parameters 258 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1148 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1788 _refine_ls_wR_factor_gt 0.1569 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.10993(5) -0.00175(3) 0.42496(5) 0.0248(2) Uani 1 1 d . . . O1 O 0.1946(4) -0.0713(3) 0.5661(4) 0.0513(11) Uani 1 1 d . . . O2 O 0.0248(4) -0.0737(3) 0.6711(4) 0.0511(11) Uani 1 1 d . . . O3 O -0.0777(6) -0.1959(4) 0.8433(7) 0.0881(19) Uani 1 1 d D . . H3 H -0.115(13) -0.157(6) 0.875(12) 0.18(6) Uiso 1 1 d D . . O4 O 0.0596(6) -0.1013(4) 0.9344(5) 0.093(2) Uani 1 1 d . . . O5 O 0.3162(4) -0.4074(2) 0.9734(4) 0.0492(11) Uani 1 1 d . . . O6 O 0.4850(4) -0.4043(2) 0.8665(4) 0.0467(10) Uani 1 1 d . . . N1 N 0.2550(4) -0.0207(2) 0.3204(4) 0.0326(10) Uani 1 1 d . . . N2 N 0.7482(7) -0.1349(5) -0.0278(6) 0.0748(19) Uani 1 1 d . . . C1 C 0.3788(8) 0.0040(6) 0.3459(10) 0.106(4) Uani 1 1 d . . . H1 H 0.4005 0.0388 0.4104 0.127 Uiso 1 1 calc R . . C2 C 0.4818(9) -0.0169(6) 0.2854(10) 0.107(4) Uani 1 1 d . . . H2 H 0.5711 0.0010 0.3121 0.129 Uiso 1 1 calc R . . C3 C 0.4539(6) -0.0636(3) 0.1865(5) 0.0396(13) Uani 1 1 d . . . C4 C 0.3181(8) -0.0830(5) 0.1511(8) 0.080(3) Uani 1 1 d . . . H4 H 0.2915 -0.1129 0.0817 0.096 Uiso 1 1 calc R . . C5 C 0.2215(7) -0.0590(5) 0.2165(7) 0.070(2) Uani 1 1 d . . . H5 H 0.1292 -0.0698 0.1874 0.083 Uiso 1 1 calc R . . C6 C 0.5580(6) -0.0867(4) 0.1141(5) 0.0463(14) Uani 1 1 d . . . C7 C 0.6787(7) -0.0448(5) 0.1164(7) 0.0626(19) Uani 1 1 d . . . H7 H 0.6981 0.0001 0.1647 0.075 Uiso 1 1 calc R . . C8 C 0.7727(7) -0.0719(5) 0.0427(8) 0.068(2) Uani 1 1 d . . . H8 H 0.8547 -0.0442 0.0444 0.082 Uiso 1 1 calc R . . C9 C 0.6343(9) -0.1757(7) -0.0259(8) 0.094(3) Uani 1 1 d . . . H9 H 0.6185 -0.2219 -0.0718 0.113 Uiso 1 1 calc R . . C10 C 0.5374(8) -0.1520(6) 0.0421(8) 0.079(3) Uani 1 1 d . . . H10 H 0.4568 -0.1814 0.0385 0.094 Uiso 1 1 calc R . . C11 C 0.1364(5) -0.0980(3) 0.6470(5) 0.0327(11) Uani 1 1 d . . . C12 C 0.2045(5) -0.1660(3) 0.7206(5) 0.0352(12) Uani 1 1 d . . . C13 C 0.1495(6) -0.1975(3) 0.8145(5) 0.0414(13) Uani 1 1 d . . . C14 C 0.0387(8) -0.1575(4) 0.8710(7) 0.0595(18) Uani 1 1 d . . . C15 C 0.2063(6) -0.2665(3) 0.8706(5) 0.0387(13) Uani 1 1 d . . . H15 H 0.1683 -0.2887 0.9328 0.046 Uiso 1 1 calc R . . C16 C 0.3194(5) -0.3029(3) 0.8347(5) 0.0350(12) Uani 1 1 d . . . C17 C 0.3781(5) -0.3779(3) 0.8956(5) 0.0319(11) Uani 1 1 d . . . C18 C 0.3757(6) -0.2697(3) 0.7432(5) 0.0398(13) Uani 1 1 d . . . H18 H 0.4528 -0.2926 0.7201 0.048 Uiso 1 1 calc R . . C19 C 0.3179(6) -0.2025(3) 0.6859(5) 0.0388(13) Uani 1 1 d . . . H19 H 0.3552 -0.1811 0.6227 0.047 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 0.0236(3) 0.0221(3) 0.0288(3) -0.0001(3) 0.00433(19) 0.0007(3) O1 0.052(3) 0.053(3) 0.048(3) 0.022(2) 0.005(2) 0.016(2) O2 0.045(2) 0.053(3) 0.055(3) 0.020(2) 0.009(2) 0.023(2) O3 0.068(4) 0.074(4) 0.133(6) -0.003(4) 0.047(4) 0.014(3) O4 0.088(4) 0.108(5) 0.083(4) -0.031(4) 0.015(3) 0.039(4) O5 0.053(3) 0.041(2) 0.057(3) 0.021(2) 0.019(2) 0.018(2) O6 0.044(2) 0.040(2) 0.057(3) 0.017(2) 0.011(2) 0.0180(18) N1 0.032(2) 0.034(2) 0.033(2) -0.0045(17) 0.0088(18) -0.0020(17) N2 0.063(4) 0.105(5) 0.062(4) 0.004(4) 0.025(3) 0.030(4) C1 0.056(5) 0.135(8) 0.142(9) -0.102(7) 0.061(5) -0.055(5) C2 0.050(4) 0.154(9) 0.129(8) -0.087(7) 0.045(5) -0.045(5) C3 0.031(3) 0.051(3) 0.041(3) -0.001(3) 0.017(2) 0.003(2) C4 0.064(5) 0.108(6) 0.078(5) -0.040(5) 0.035(4) -0.027(5) C5 0.045(4) 0.093(6) 0.075(5) -0.032(4) 0.025(4) -0.022(4) C6 0.034(3) 0.064(4) 0.044(3) -0.004(3) 0.015(3) 0.009(3) C7 0.045(4) 0.076(5) 0.074(5) 0.001(4) 0.030(3) 0.004(4) C8 0.042(4) 0.083(5) 0.084(6) 0.027(5) 0.027(4) 0.006(4) C9 0.057(5) 0.144(9) 0.089(6) -0.051(6) 0.030(5) 0.010(6) C10 0.045(4) 0.115(7) 0.081(5) -0.042(5) 0.026(4) -0.002(4) C11 0.038(3) 0.026(2) 0.032(3) 0.001(2) -0.002(2) 0.003(2) C12 0.036(3) 0.029(3) 0.041(3) 0.008(2) 0.008(2) 0.011(2) C13 0.038(3) 0.039(3) 0.050(4) 0.011(3) 0.012(3) 0.018(2) C14 0.057(4) 0.052(4) 0.069(5) 0.009(4) 0.013(4) 0.019(4) C15 0.042(3) 0.039(3) 0.038(3) 0.013(2) 0.016(3) 0.013(2) C16 0.033(3) 0.027(2) 0.044(3) 0.007(2) 0.005(2) 0.007(2) C17 0.029(3) 0.024(2) 0.038(3) -0.001(2) -0.005(2) 0.006(2) C18 0.036(3) 0.036(3) 0.052(4) 0.012(3) 0.019(3) 0.016(2) C19 0.040(3) 0.041(3) 0.037(3) 0.011(2) 0.012(2) 0.012(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 2.012(4) 3_556 ? Zn1 O5 2.017(4) 2_556 ? Zn1 N1 2.034(4) . ? Zn1 O1 2.034(4) . ? Zn1 O6 2.040(4) 4 ? Zn1 Zn1 2.9779(13) 3_556 ? O1 C11 1.245(6) . ? O2 C11 1.249(6) . ? O2 Zn1 2.012(4) 3_556 ? O3 C14 1.307(9) . ? O4 C14 1.180(9) . ? O5 C17 1.256(7) . ? O5 Zn1 2.017(4) 2_546 ? O6 C17 1.240(6) . ? O6 Zn1 2.040(4) 4_656 ? N1 C1 1.275(8) . ? N1 C5 1.329(8) . ? N2 C8 1.319(10) . ? N2 C9 1.321(11) . ? C1 C2 1.366(10) . ? C2 C3 1.353(10) . ? C3 C4 1.369(9) . ? C3 C6 1.473(7) . ? C4 C5 1.365(10) . ? C6 C10 1.359(9) . ? C6 C7 1.380(9) . ? C7 C8 1.425(9) . ? C9 C10 1.385(9) . ? C11 C12 1.499(7) . ? C12 C13 1.379(7) . ? C12 C19 1.391(7) . ? C13 C15 1.390(7) . ? C13 C14 1.516(8) . ? C15 C16 1.393(7) . ? C16 C18 1.374(7) . ? C16 C17 1.502(7) . ? C18 C19 1.374(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 O2 Zn1 O5 87.3(2) 3_556 2_556 ? O2 Zn1 N1 104.54(18) 3_556 . ? O5 Zn1 N1 103.46(17) 2_556 . ? O2 Zn1 O1 157.91(18) 3_556 . ? O5 Zn1 O1 86.86(19) 2_556 . ? N1 Zn1 O1 97.54(18) . . ? O2 Zn1 O6 90.36(19) 3_556 4 ? O5 Zn1 O6 158.41(17) 2_556 4 ? N1 Zn1 O6 97.90(17) . 4 ? O1 Zn1 O6 87.31(18) . 4 ? O2 Zn1 Zn1 79.41(12) 3_556 3_556 ? O5 Zn1 Zn1 83.52(12) 2_556 3_556 ? N1 Zn1 Zn1 172.01(12) . 3_556 ? O1 Zn1 Zn1 78.77(13) . 3_556 ? O6 Zn1 Zn1 74.96(12) 4 3_556 ? C11 O1 Zn1 127.2(4) . . ? C11 O2 Zn1 127.9(4) . 3_556 ? C17 O5 Zn1 122.4(3) . 2_546 ? C17 O6 Zn1 133.2(4) . 4_656 ? C1 N1 C5 116.0(6) . . ? C1 N1 Zn1 124.2(5) . . ? C5 N1 Zn1 119.8(4) . . ? C8 N2 C9 118.3(7) . . ? N1 C1 C2 124.8(7) . . ? C3 C2 C1 119.9(7) . . ? C2 C3 C4 115.3(6) . . ? C2 C3 C6 123.3(6) . . ? C4 C3 C6 121.1(6) . . ? C5 C4 C3 120.8(7) . . ? N1 C5 C4 122.0(7) . . ? C10 C6 C7 117.5(6) . . ? C10 C6 C3 119.9(6) . . ? C7 C6 C3 122.6(6) . . ? C6 C7 C8 118.3(7) . . ? N2 C8 C7 122.6(7) . . ? N2 C9 C10 122.1(9) . . ? C6 C10 C9 121.2(8) . . ? O1 C11 O2 125.4(5) . . ? O1 C11 C12 117.6(5) . . ? O2 C11 C12 117.1(5) . . ? C13 C12 C19 119.4(5) . . ? C13 C12 C11 121.4(5) . . ? C19 C12 C11 118.9(5) . . ? C12 C13 C15 119.3(5) . . ? C12 C13 C14 124.3(5) . . ? C15 C13 C14 116.1(5) . . ? O4 C14 O3 126.4(7) . . ? O4 C14 C13 123.1(7) . . ? O3 C14 C13 110.4(7) . . ? C13 C15 C16 120.8(5) . . ? C18 C16 C15 119.4(5) . . ? C18 C16 C17 120.7(5) . . ? C15 C16 C17 119.9(5) . . ? O6 C17 O5 125.8(5) . . ? O6 C17 C16 117.1(5) . . ? O5 C17 C16 117.1(4) . . ? C19 C18 C16 119.9(5) . . ? C18 C19 C12 121.1(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 N2 0.852(10) 1.92(9) 2.645(8) 142(13) 1_456 _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.988 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.104