Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 X-Sun-Charset: us-ascii X-Sun-Content-Lines: 499 data_global #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Chen, Xiao-Ming School of Chemistry and Chemical Engineering Zhongshan University Guangzhou, 510275 P. R. China ; _publ_contact_author_phone '86 20 84113986' _publ_contact_author_fax '86 20 84112245' _publ_contact_author_email cescxm@zsu.edu.cn _publ_requested_joiurnal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as supplmentary data for a manuscript submitted to J. Chem. Soc., Dalton Trans. Xiao-Ming Chen ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_Cambridge 186 _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; A Novel Polycatenated Double-layered Hybrid Organic-inorganic Material Constructed From [Zn2(tp)(4,4-bpy)]n2n+ Layers and V2O62- Pillars ; loop_ _publ_author_name _publ_author_address 'Tao Jun' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Zhang, Xian-Ming' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Tong, Ming-Liang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Chen, Xiao-Ming' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China #============================================================ data_complex_1 _database_code_CSD 155435 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 N2 O10 V2 Zn2' _chemical_formula_weight 648.92 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' 'V' 'V' 0.3005 0.5294 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.537(6) _cell_length_b 10.760(6) _cell_length_c 11.272(8) _cell_angle_alpha 80.660(10) _cell_angle_beta 63.27(2) _cell_angle_gamma 63.860(10) _cell_volume 1023.7(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour light yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 3.263 _exptl_absorpt_correction_type \y-scan _exptl_absorpt_correction_T_min 0.3553 _exptl_absorpt_correction_T_max 0.4619 _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 R3m' _diffrn_measurement_method '\w scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 4990 _diffrn_reflns_av_R_equivalents 0.0139 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 29.85 _reflns_number_total 4929 _reflns_number_gt 3759 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+1.1824P] 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 0.0062(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4929 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1316 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.28873(6) 0.50316(5) 0.28303(5) 0.02719(15) Uani 1 d . . . Zn2 Zn 0.25238(6) 0.77126(5) 0.09817(5) 0.03090(16) Uani 1 d . . . V3 V 0.15873(9) 1.03819(8) 0.28532(7) 0.03010(19) Uani 1 d . . . V4 V 0.19975(9) 0.77012(7) 0.46156(8) 0.02947(18) Uani 1 d . . . N1 N 0.2975(4) 0.3537(4) 0.4149(4) 0.0293(7) Uani 1 d . . . N2 N 0.3014(4) -0.1447(4) 0.9125(4) 0.0317(8) Uani 1 d . . . O1 O 0.1517(4) 0.4949(3) 0.2146(3) 0.0331(7) Uani 1 d . . . O2 O 0.1161(4) 0.6914(3) 0.1020(3) 0.0345(7) Uani 1 d . . . O3 O -0.5358(4) 0.6875(4) 0.0893(3) 0.0366(7) Uani 1 d . . . O4 O -0.4943(4) 0.4831(3) 0.1858(3) 0.0355(7) Uani 1 d . . . O5 O 0.1280(4) 0.9495(4) 0.1990(4) 0.0447(8) Uani 1 d . . . O6 O -0.0222(5) 1.1730(4) 0.3907(4) 0.0555(10) Uani 1 d . . . O7 O 0.2782(5) 1.1034(5) 0.1851(4) 0.0574(11) Uani 1 d . . . O8 O 0.2470(4) 0.9140(3) 0.3861(3) 0.0394(8) Uani 1 d . . . O9 O 0.3400(4) 0.6582(4) 0.4962(4) 0.0455(9) Uani 1 d . . . O10 O 0.1808(4) 0.6948(3) 0.3518(4) 0.0441(8) Uani 1 d . . . C1 C 0.0802(5) 0.5918(4) 0.1561(4) 0.0246(8) Uani 1 d . . . C2 C -0.0576(4) 0.5878(4) 0.1485(4) 0.0229(8) Uani 1 d . . . C3 C -0.1125(5) 0.4879(4) 0.2159(4) 0.0278(8) Uani 1 d . . . H3A H -0.0616 0.4213 0.2660 0.080 Uiso 1 d R . . C4 C -0.2398(5) 0.4844(4) 0.2110(4) 0.0278(8) Uani 1 d . . . H4A H -0.2760 0.4146 0.2561 0.080 Uiso 1 d R . . C5 C -0.3159(4) 0.5834(4) 0.1391(4) 0.0232(8) Uani 1 d . . . C6 C -0.2621(5) 0.6838(4) 0.0727(4) 0.0268(8) Uani 1 d . . . H6A H -0.3143 0.7517 0.0242 0.080 Uiso 1 d R . . C7 C -0.1330(5) 0.6849(4) 0.0773(4) 0.0254(8) Uani 1 d . . . H7A H -0.0951 0.7533 0.0306 0.080 Uiso 1 d R . . C8 C -0.4582(5) 0.5841(4) 0.1375(4) 0.0253(8) Uani 1 d . . . C9 C 0.1986(6) 0.2922(5) 0.4561(5) 0.0410(11) Uani 1 d . . . H9A H 0.1222 0.3212 0.4213 0.080 Uiso 1 d R . . C10 C 0.2034(6) 0.1886(5) 0.5475(5) 0.0362(10) Uani 1 d . . . H10A H 0.1315 0.1465 0.5746 0.080 Uiso 1 d R . . C11 C 0.3138(5) 0.1448(4) 0.6005(4) 0.0254(8) Uani 1 d . . . C12 C 0.4141(5) 0.2101(5) 0.5572(5) 0.0328(9) Uani 1 d . . . H12A H 0.4914 0.1839 0.5905 0.080 Uiso 1 d R . . C13 C 0.4031(5) 0.3127(5) 0.4658(5) 0.0321(9) Uani 1 d . . . H13A H 0.4730 0.3570 0.4376 0.080 Uiso 1 d R . . C14 C 0.3172(5) 0.0372(4) 0.7025(4) 0.0260(8) Uani 1 d . . . C15 C 0.2132(6) -0.0252(5) 0.7473(5) 0.0414(12) Uani 1 d . . . H15A H 0.1450 -0.0062 0.7057 0.080 Uiso 1 d R . . C16 C 0.2081(6) -0.1133(6) 0.8504(5) 0.0435(12) Uani 1 d . . . H16A H 0.1354 -0.1549 0.8795 0.080 Uiso 1 d R . . C17 C 0.4068(5) -0.0915(5) 0.8663(5) 0.0367(10) Uani 1 d . . . H17A H 0.4769 -0.1160 0.9071 0.080 Uiso 1 d R . . C18 C 0.4186(5) -0.0007(5) 0.7623(5) 0.0361(10) Uani 1 d . . . H18A H 0.4965 0.0350 0.7316 0.080 Uiso 1 d 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 0.0277(3) 0.0295(3) 0.0372(3) 0.0110(2) -0.0210(2) -0.0184(2) Zn2 0.0275(3) 0.0301(3) 0.0469(3) 0.0122(2) -0.0226(2) -0.0184(2) V3 0.0289(4) 0.0365(4) 0.0309(4) 0.0092(3) -0.0140(3) -0.0199(3) V4 0.0300(4) 0.0285(4) 0.0380(4) 0.0041(3) -0.0183(3) -0.0158(3) N1 0.0283(18) 0.0337(19) 0.0321(19) 0.0079(15) -0.0153(15) -0.0175(15) N2 0.0296(18) 0.0334(19) 0.039(2) 0.0108(16) -0.0171(16) -0.0199(16) O1 0.0309(16) 0.0359(17) 0.0491(19) 0.0111(14) -0.0285(15) -0.0190(14) O2 0.0384(17) 0.0464(18) 0.0400(17) 0.0162(14) -0.0236(15) -0.0331(15) O3 0.0277(15) 0.0475(19) 0.0449(18) 0.0205(15) -0.0242(14) -0.0214(14) O4 0.0259(15) 0.0367(17) 0.053(2) 0.0089(15) -0.0198(15) -0.0196(13) O5 0.046(2) 0.046(2) 0.052(2) 0.0003(16) -0.0326(18) -0.0154(17) O6 0.049(2) 0.045(2) 0.053(2) -0.0005(17) -0.0094(18) -0.0148(18) O7 0.049(2) 0.082(3) 0.059(2) 0.038(2) -0.030(2) -0.048(2) O8 0.055(2) 0.0429(18) 0.0452(19) 0.0151(15) -0.0321(17) -0.0338(17) O9 0.042(2) 0.045(2) 0.064(2) 0.0136(17) -0.0338(18) -0.0225(17) O10 0.045(2) 0.0315(17) 0.070(2) -0.0034(16) -0.0345(19) -0.0157(15) C1 0.0227(19) 0.033(2) 0.0243(19) 0.0004(16) -0.0110(16) -0.0161(17) C2 0.0201(18) 0.030(2) 0.0242(18) 0.0007(15) -0.0114(15) -0.0131(16) C3 0.028(2) 0.030(2) 0.034(2) 0.0120(17) -0.0184(18) -0.0165(17) C4 0.025(2) 0.033(2) 0.033(2) 0.0087(17) -0.0134(17) -0.0203(17) C5 0.0196(18) 0.0282(19) 0.0265(19) 0.0022(15) -0.0102(15) -0.0137(15) C6 0.0239(19) 0.031(2) 0.031(2) 0.0093(17) -0.0163(17) -0.0141(17) C7 0.0235(19) 0.029(2) 0.029(2) 0.0038(16) -0.0120(16) -0.0151(16) C8 0.0207(18) 0.033(2) 0.0250(19) 0.0013(16) -0.0085(15) -0.0145(16) C9 0.044(3) 0.045(3) 0.055(3) 0.020(2) -0.032(2) -0.031(2) C10 0.043(3) 0.042(3) 0.047(3) 0.018(2) -0.030(2) -0.031(2) C11 0.026(2) 0.0261(19) 0.028(2) 0.0032(16) -0.0128(17) -0.0129(16) C12 0.030(2) 0.040(2) 0.039(2) 0.0140(19) -0.023(2) -0.0203(19) C13 0.031(2) 0.036(2) 0.043(2) 0.0139(19) -0.022(2) -0.0227(19) C14 0.0215(19) 0.030(2) 0.027(2) 0.0042(16) -0.0101(16) -0.0129(16) C15 0.044(3) 0.053(3) 0.051(3) 0.024(2) -0.032(2) -0.036(2) C16 0.048(3) 0.056(3) 0.049(3) 0.022(2) -0.029(2) -0.039(3) C17 0.035(2) 0.043(3) 0.046(3) 0.015(2) -0.025(2) -0.024(2) C18 0.033(2) 0.044(3) 0.045(3) 0.020(2) -0.024(2) -0.026(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 O10 1.950(3) . ? Zn1 O1 1.956(3) . ? Zn1 O4 1.966(3) 1_655 ? Zn1 N1 2.005(4) . ? Zn2 O2 1.955(3) . ? Zn2 O5 1.960(4) . ? Zn2 O3 1.964(3) 1_655 ? Zn2 N2 2.071(4) 1_564 ? V3 O7 1.611(3) . ? V3 O5 1.678(3) . ? V3 O6 1.799(4) . ? V3 O8 1.818(3) . ? V4 O9 1.608(3) . ? V4 O10 1.709(3) . ? V4 O6 1.779(4) 2_576 ? V4 O8 1.800(3) . ? N1 C9 1.346(5) . ? N1 C13 1.349(5) . ? N2 C17 1.333(5) . ? N2 C16 1.349(6) . ? N2 Zn2 2.071(4) 1_546 ? O1 C1 1.273(5) . ? O2 C1 1.265(5) . ? O3 C8 1.266(5) . ? O3 Zn2 1.964(3) 1_455 ? O4 C8 1.269(5) . ? O4 Zn1 1.966(3) 1_455 ? O6 V4 1.779(4) 2_576 ? C1 C2 1.511(5) . ? C2 C7 1.392(5) . ? C2 C3 1.399(5) . ? C3 C4 1.384(5) . ? C4 C5 1.409(6) . ? C5 C6 1.394(5) . ? C5 C8 1.505(5) . ? C6 C7 1.390(5) . ? C9 C10 1.390(6) . ? C10 C11 1.408(6) . ? C11 C12 1.389(6) . ? C11 C14 1.494(6) . ? C12 C13 1.385(6) . ? C14 C18 1.392(6) . ? C14 C15 1.396(6) . ? C15 C16 1.372(6) . ? C17 C18 1.395(6) . ? 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 O10 Zn1 O1 101.84(14) . . ? O10 Zn1 O4 101.23(14) . 1_655 ? O1 Zn1 O4 129.17(15) . 1_655 ? O10 Zn1 N1 117.62(16) . . ? O1 Zn1 N1 103.81(14) . . ? O4 Zn1 N1 104.41(14) 1_655 . ? O2 Zn2 O5 110.46(15) . . ? O2 Zn2 O3 132.50(15) . 1_655 ? O5 Zn2 O3 110.65(15) . 1_655 ? O2 Zn2 N2 100.18(13) . 1_564 ? O5 Zn2 N2 95.58(16) . 1_564 ? O3 Zn2 N2 98.51(14) 1_655 1_564 ? O7 V3 O5 110.1(2) . . ? O7 V3 O6 110.1(2) . . ? O5 V3 O6 111.0(2) . . ? O7 V3 O8 109.13(18) . . ? O5 V3 O8 106.55(17) . . ? O6 V3 O8 109.89(19) . . ? O9 V4 O10 108.94(18) . . ? O9 V4 O6 109.8(2) . 2_576 ? O10 V4 O6 109.6(2) . 2_576 ? O9 V4 O8 108.77(17) . . ? O10 V4 O8 109.29(17) . . ? O6 V4 O8 110.46(18) 2_576 . ? C9 N1 C13 118.0(4) . . ? C9 N1 Zn1 121.5(3) . . ? C13 N1 Zn1 120.5(3) . . ? C17 N2 C16 117.5(4) . . ? C17 N2 Zn2 118.5(3) . 1_546 ? C16 N2 Zn2 122.3(3) . 1_546 ? C1 O1 Zn1 125.3(3) . . ? C1 O2 Zn2 137.3(3) . . ? C8 O3 Zn2 136.4(3) . 1_455 ? C8 O4 Zn1 123.3(3) . 1_455 ? V3 O5 Zn2 134.5(2) . . ? V4 O6 V3 151.2(3) 2_576 . ? V4 O8 V3 124.70(18) . . ? V4 O10 Zn1 129.7(2) . . ? O2 C1 O1 125.2(4) . . ? O2 C1 C2 116.8(3) . . ? O1 C1 C2 118.0(3) . . ? C7 C2 C3 119.5(3) . . ? C7 C2 C1 120.5(3) . . ? C3 C2 C1 119.9(3) . . ? C4 C3 C2 120.4(4) . . ? C3 C4 C5 119.8(4) . . ? C6 C5 C4 119.9(3) . . ? C6 C5 C8 119.8(3) . . ? C4 C5 C8 120.3(3) . . ? C7 C6 C5 119.6(4) . . ? C6 C7 C2 120.8(4) . . ? O3 C8 O4 124.2(4) . . ? O3 C8 C5 117.4(4) . . ? O4 C8 C5 118.4(4) . . ? N1 C9 C10 122.1(4) . . ? C9 C10 C11 120.2(4) . . ? C12 C11 C10 116.8(4) . . ? C12 C11 C14 122.1(4) . . ? C10 C11 C14 121.1(4) . . ? C13 C12 C11 120.0(4) . . ? N1 C13 C12 122.9(4) . . ? C18 C14 C15 116.7(4) . . ? C18 C14 C11 121.8(4) . . ? C15 C14 C11 121.4(4) . . ? C16 C15 C14 120.3(4) . . ? N2 C16 C15 122.8(4) . . ? N2 C17 C18 122.9(4) . . ? C14 C18 C17 119.6(4) . . ? _diffrn_measured_fraction_theta_max 0.840 _diffrn_reflns_theta_full 29.85 _diffrn_measured_fraction_theta_full 0.840 _refine_diff_density_max 0.662 _refine_diff_density_min -1.122 _refine_diff_density_rms 0.124 #_eof #End of Crystallographic Information File