# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Zhengbo Han' _publ_contact_author_address ; College of Chemistry Liaoning Uniersity 66 Chongshan Rd. M., Shenyang 110036, China Shenyang 110036 CHINA ; _publ_contact_author_email CESHZB@LNU.EDU.CN _publ_section_title ; A 3D chiral Zn(II) coordination polymer with triple Zn-oba-Zn helical chains (oba = 4,4'-oxybis(benzoate)) ; loop_ _publ_author_name 'Zhengbo Han.' 'Yong-Ke He.' 'Yi Ma.' 'Liguo Yang.' data_1 _database_code_depnum_ccdc_archive 'CCDC 649445' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H16 N0 O10 Zn2' _chemical_formula_weight 643.15 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 Trigonal _symmetry_space_group_name_H-M P3(2)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' _cell_length_a 13.298(2) _cell_length_b 13.298(2) _cell_length_c 29.544(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4524.5(12) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 1.641 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.5189 _exptl_absorpt_correction_T_max 0.6656 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8644 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0649 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6834 _reflns_number_gt 4658 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS (Siemens, 1994)' _computing_cell_refinement 'XSCANS (Siemens, 1994)' _computing_data_reduction 'XSCANS (Siemens, 1994)' _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^)+(0.1362P)^2^+4.4498P] 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 SHELXL _refine_ls_extinction_coef 0.0132(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 6834 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1153 _refine_ls_R_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.2357 _refine_ls_wR_factor_gt 0.1936 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 0.46553(10) 0.46537(10) 0.10652(3) 0.0638(3) Uani 1 1 d . . . Zn2 Zn 0.28176(8) 0.44995(9) 0.18455(3) 0.0514(3) Uani 1 1 d . . . C1 C 0.5098(8) 0.6461(8) 0.1781(3) 0.060(2) Uani 1 1 d . . . C2 C 0.6010(8) 0.7531(8) 0.1983(3) 0.0590(19) Uani 1 1 d . . . C3 C 0.7176(8) 0.7936(8) 0.1869(3) 0.063(2) Uani 1 1 d . . . H3A H 0.7360 0.7537 0.1657 0.076 Uiso 1 1 calc R . . C4 C 0.8037(9) 0.8908(9) 0.2069(3) 0.069(2) Uani 1 1 d . . . H4A H 0.8806 0.9164 0.1991 0.083 Uiso 1 1 calc R . . C5 C 0.7793(9) 0.9518(8) 0.2383(3) 0.070(2) Uani 1 1 d . . . C6 C 0.6664(9) 0.9136(9) 0.2504(4) 0.085(3) Uani 1 1 d . . . H6A H 0.6494 0.9537 0.2720 0.102 Uiso 1 1 calc R . . C7 C 0.5777(9) 0.8152(9) 0.2303(4) 0.080(3) Uani 1 1 d . . . H7A H 0.5012 0.7902 0.2383 0.096 Uiso 1 1 calc R . . C8 C 0.8521(8) 1.1072(8) 0.2914(3) 0.069(2) Uani 1 1 d . . . C9 C 0.8416(11) 1.0609(8) 0.3348(4) 0.094(4) Uani 1 1 d . . . H9A H 0.8375 0.9899 0.3398 0.113 Uiso 1 1 calc R . . C10 C 0.8378(10) 1.1287(8) 0.3703(4) 0.082(3) Uani 1 1 d . . . H10A H 0.8308 1.1017 0.3998 0.099 Uiso 1 1 calc R . . C11 C 0.8439(6) 1.2328(6) 0.3631(2) 0.0483(16) Uani 1 1 d . . . C12 C 0.8526(8) 1.2720(8) 0.3197(2) 0.059(2) Uani 1 1 d . . . H12A H 0.8575 1.3432 0.3143 0.071 Uiso 1 1 calc R . . C13 C 0.8541(9) 1.2062(8) 0.2842(3) 0.075(3) Uani 1 1 d . . . H13A H 0.8566 1.2318 0.2547 0.091 Uiso 1 1 calc R . . C14 C 0.8648(6) 1.3125(7) 0.4021(3) 0.0484(17) Uani 1 1 d . . . C15 C 0.2185(10) -0.2539(8) 0.4212(3) 0.067(2) Uani 1 1 d . . . C16 C 0.3063(10) -0.1764(8) 0.3867(3) 0.066(2) Uani 1 1 d . . . C17 C 0.3988(10) -0.0743(9) 0.3997(3) 0.079(3) Uani 1 1 d . . . H17A H 0.4103 -0.0562 0.4303 0.095 Uiso 1 1 calc R . . C18 C 0.4775(12) 0.0045(12) 0.3685(4) 0.099(4) Uani 1 1 d . . . H18A H 0.5406 0.0744 0.3778 0.119 Uiso 1 1 calc R . . C19 C 0.4587(12) -0.0244(13) 0.3245(4) 0.096(4) Uani 1 1 d . . . C20 C 0.3704(14) -0.1311(13) 0.3107(4) 0.100(4) Uani 1 1 d . . . H20A H 0.3626 -0.1507 0.2802 0.119 Uiso 1 1 calc R . . C21 C 0.2941(13) -0.2084(12) 0.3413(3) 0.097(4) Uani 1 1 d . . . H21A H 0.2351 -0.2809 0.3320 0.116 Uiso 1 1 calc R . . C22 C 0.4938(11) 0.1092(12) 0.2659(4) 0.097(4) Uani 1 1 d . . . C23 C 0.4084(14) 0.1283(15) 0.2802(5) 0.130(7) Uani 1 1 d . . . H23A H 0.3696 0.0955 0.3071 0.155 Uiso 1 1 calc R . . C24 C 0.3789(13) 0.1971(14) 0.2547(4) 0.114(5) Uani 1 1 d . . . H24A H 0.3233 0.2138 0.2656 0.137 Uiso 1 1 calc R . . C25 C 0.4302(9) 0.2411(8) 0.2135(3) 0.070(3) Uani 1 1 d . . . C26 C 0.5214(11) 0.2207(11) 0.1996(4) 0.091(4) Uani 1 1 d . . . H26A H 0.5604 0.2515 0.1724 0.109 Uiso 1 1 calc R . . C27 C 0.5508(11) 0.1566(12) 0.2259(4) 0.101(5) Uani 1 1 d . . . H27A H 0.6107 0.1443 0.2169 0.122 Uiso 1 1 calc R . . C28 C 0.3985(9) 0.3125(8) 0.1848(3) 0.067(2) Uani 1 1 d . . . O1 O 0.5343(6) 0.6066(7) 0.1454(2) 0.082(2) Uani 1 1 d . . . O2 O 0.4113(6) 0.6018(6) 0.1966(2) 0.082(2) Uani 1 1 d . . . O3 O 0.8710(7) 1.0488(6) 0.2554(3) 0.101(3) Uani 1 1 d . . . O4 O 0.9151(5) 1.4209(5) 0.39358(18) 0.0557(13) Uani 1 1 d . . . O5 O 0.8388(6) 1.2732(6) 0.44181(19) 0.0729(18) Uani 1 1 d . . . O6 O 0.1415(8) -0.3510(6) 0.4088(2) 0.099(3) Uani 1 1 d . . . O7 O 0.2267(6) -0.2129(6) 0.45973(18) 0.0703(18) Uani 1 1 d . . . O8 O 0.5347(8) 0.0501(9) 0.2910(3) 0.120(4) Uani 1 1 d . . . O9 O 0.3245(7) 0.3350(7) 0.2002(2) 0.085(2) Uani 1 1 d . . . O10 O 0.4440(7) 0.3435(6) 0.1469(2) 0.080(2) Uani 1 1 d . . . 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 0.0778(7) 0.0816(7) 0.0475(5) 0.0172(5) 0.0214(5) 0.0515(7) Zn2 0.0500(5) 0.0675(6) 0.0409(4) 0.0047(4) 0.0037(4) 0.0325(5) C1 0.058(5) 0.058(5) 0.065(5) -0.009(4) -0.011(4) 0.028(4) C2 0.059(5) 0.063(5) 0.061(4) -0.010(4) -0.002(4) 0.036(4) C3 0.068(6) 0.067(5) 0.060(5) -0.008(4) 0.007(4) 0.038(5) C4 0.060(5) 0.066(6) 0.076(6) -0.008(5) 0.015(5) 0.028(5) C5 0.083(6) 0.047(4) 0.075(5) -0.013(4) 0.017(5) 0.028(5) C6 0.067(6) 0.065(6) 0.119(9) -0.027(6) 0.020(6) 0.030(5) C7 0.063(6) 0.080(7) 0.107(8) -0.031(6) 0.003(5) 0.044(5) C8 0.057(5) 0.052(5) 0.071(6) -0.017(4) 0.012(4) 0.008(4) C9 0.112(9) 0.044(5) 0.117(9) 0.004(5) 0.055(8) 0.032(6) C10 0.094(7) 0.055(6) 0.087(7) 0.014(5) 0.036(6) 0.030(5) C11 0.041(4) 0.044(4) 0.045(3) -0.002(3) 0.003(3) 0.010(3) C12 0.062(5) 0.056(5) 0.044(4) -0.008(3) -0.009(4) 0.018(4) C13 0.083(7) 0.061(6) 0.045(4) -0.009(4) 0.006(4) 0.009(5) C14 0.040(4) 0.050(4) 0.049(4) -0.003(3) -0.001(3) 0.017(3) C15 0.097(7) 0.058(5) 0.046(4) 0.003(4) 0.006(4) 0.037(5) C16 0.096(7) 0.060(5) 0.050(4) 0.011(4) 0.015(4) 0.046(5) C17 0.092(7) 0.070(6) 0.070(6) 0.019(5) 0.019(5) 0.035(6) C18 0.099(9) 0.095(8) 0.103(9) 0.031(7) 0.036(7) 0.049(7) C19 0.119(10) 0.115(10) 0.099(8) 0.061(8) 0.058(8) 0.092(9) C20 0.144(12) 0.117(10) 0.060(6) 0.026(7) 0.043(7) 0.082(10) C21 0.149(12) 0.092(8) 0.052(5) 0.006(5) 0.030(6) 0.062(8) C22 0.109(9) 0.123(10) 0.103(8) 0.067(8) 0.053(7) 0.092(8) C23 0.148(12) 0.181(15) 0.129(10) 0.111(11) 0.104(10) 0.134(12) C24 0.139(11) 0.167(13) 0.105(8) 0.079(9) 0.076(8) 0.128(11) C25 0.081(6) 0.074(6) 0.073(6) 0.026(5) 0.037(5) 0.051(5) C26 0.106(9) 0.097(8) 0.089(7) 0.039(6) 0.052(7) 0.066(7) C27 0.110(9) 0.121(10) 0.126(9) 0.064(8) 0.066(8) 0.097(9) C28 0.071(6) 0.071(6) 0.072(5) 0.018(5) 0.013(5) 0.045(5) O1 0.072(4) 0.109(6) 0.063(4) -0.030(4) -0.005(3) 0.044(4) O2 0.061(4) 0.075(4) 0.087(5) -0.022(4) -0.002(4) 0.017(3) O3 0.073(4) 0.075(5) 0.107(6) -0.044(4) 0.029(4) 0.000(4) O4 0.060(3) 0.051(3) 0.049(3) -0.006(2) -0.004(2) 0.022(3) O5 0.071(4) 0.075(4) 0.042(3) 0.005(3) 0.007(3) 0.013(3) O6 0.144(7) 0.051(4) 0.052(3) -0.003(3) 0.017(4) 0.011(4) O7 0.084(4) 0.070(4) 0.039(3) 0.001(3) 0.005(3) 0.025(3) O8 0.120(7) 0.156(8) 0.141(7) 0.103(7) 0.084(6) 0.111(7) O9 0.099(5) 0.112(6) 0.079(4) 0.031(4) 0.033(4) 0.078(5) O10 0.106(5) 0.075(4) 0.074(4) 0.019(3) 0.026(4) 0.055(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 O10 1.915(7) . ? Zn1 O4 1.928(5) 2_764 ? Zn1 O6 1.960(8) 2_554 ? Zn1 O1 1.991(7) . ? Zn2 O7 1.919(6) 2_554 ? Zn2 O2 1.922(7) . ? Zn2 O5 1.924(6) 6_655 ? Zn2 O9 1.935(7) . ? C1 O1 1.221(11) . ? C1 O2 1.260(12) . ? C1 C2 1.458(12) . ? C2 C7 1.387(12) . ? C2 C3 1.405(12) . ? C3 C4 1.360(13) . ? C4 C5 1.374(12) . ? C5 O3 1.353(11) . ? C5 C6 1.370(14) . ? C6 C7 1.384(14) . ? C8 C13 1.321(14) . ? C8 C9 1.400(16) . ? C8 O3 1.411(11) . ? C9 C10 1.400(14) . ? C10 C11 1.362(13) . ? C11 C12 1.368(10) . ? C11 C14 1.494(10) . ? C12 C13 1.373(12) . ? C14 O5 1.260(9) . ? C14 O4 1.274(10) . ? C15 O6 1.236(12) . ? C15 O7 1.244(10) . ? C15 C16 1.502(13) . ? C16 C17 1.354(15) . ? C16 C21 1.393(13) . ? C17 C18 1.394(15) . ? C18 C19 1.343(18) . ? C19 C20 1.38(2) . ? C19 O8 1.407(12) . ? C20 C21 1.364(16) . ? C22 C23 1.351(14) . ? C22 C27 1.374(14) . ? C22 O8 1.375(12) . ? C23 C24 1.385(15) . ? C24 C25 1.375(12) . ? C25 C26 1.429(13) . ? C25 C28 1.483(13) . ? C26 C27 1.348(15) . ? C28 O10 1.242(11) . ? C28 O9 1.249(11) . ? O4 Zn1 1.928(5) 3_675 ? O5 Zn2 1.924(6) 6_665 ? O6 Zn1 1.960(8) 3 ? O7 Zn2 1.919(6) 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 O10 Zn1 O4 112.4(3) . 2_764 ? O10 Zn1 O6 130.3(3) . 2_554 ? O4 Zn1 O6 103.6(3) 2_764 2_554 ? O10 Zn1 O1 104.1(3) . . ? O4 Zn1 O1 106.0(3) 2_764 . ? O6 Zn1 O1 97.4(4) 2_554 . ? O7 Zn2 O2 112.7(3) 2_554 . ? O7 Zn2 O5 101.8(3) 2_554 6_655 ? O2 Zn2 O5 105.0(3) . 6_655 ? O7 Zn2 O9 118.4(3) 2_554 . ? O2 Zn2 O9 108.8(4) . . ? O5 Zn2 O9 109.0(3) 6_655 . ? O1 C1 O2 125.5(9) . . ? O1 C1 C2 118.2(9) . . ? O2 C1 C2 116.2(8) . . ? C7 C2 C3 117.8(8) . . ? C7 C2 C1 122.3(9) . . ? C3 C2 C1 119.8(8) . . ? C4 C3 C2 120.3(8) . . ? C3 C4 C5 121.3(9) . . ? O3 C5 C6 123.6(8) . . ? O3 C5 C4 116.7(9) . . ? C6 C5 C4 119.7(9) . . ? C5 C6 C7 119.8(9) . . ? C6 C7 C2 121.2(9) . . ? C13 C8 C9 122.2(9) . . ? C13 C8 O3 120.5(10) . . ? C9 C8 O3 117.0(9) . . ? C10 C9 C8 115.5(10) . . ? C11 C10 C9 122.4(10) . . ? C10 C11 C12 118.9(8) . . ? C10 C11 C14 119.8(8) . . ? C12 C11 C14 120.1(7) . . ? C11 C12 C13 120.0(9) . . ? C8 C13 C12 120.9(9) . . ? O5 C14 O4 122.2(7) . . ? O5 C14 C11 120.5(7) . . ? O4 C14 C11 117.2(7) . . ? O6 C15 O7 125.0(9) . . ? O6 C15 C16 118.0(8) . . ? O7 C15 C16 116.9(9) . . ? C17 C16 C21 119.1(10) . . ? C17 C16 C15 120.1(8) . . ? C21 C16 C15 120.8(10) . . ? C16 C17 C18 122.1(11) . . ? C19 C18 C17 117.5(13) . . ? C18 C19 C20 121.5(10) . . ? C18 C19 O8 120.9(15) . . ? C20 C19 O8 117.4(13) . . ? C21 C20 C19 120.7(12) . . ? C20 C21 C16 118.7(13) . . ? C23 C22 C27 120.3(9) . . ? C23 C22 O8 123.3(9) . . ? C27 C22 O8 116.3(9) . . ? C22 C23 C24 119.8(9) . . ? C25 C24 C23 121.2(10) . . ? C24 C25 C26 117.5(9) . . ? C24 C25 C28 122.6(9) . . ? C26 C25 C28 119.8(8) . . ? C27 C26 C25 119.6(9) . . ? C26 C27 C22 121.4(9) . . ? O10 C28 O9 124.2(8) . . ? O10 C28 C25 118.7(8) . . ? O9 C28 C25 117.1(8) . . ? C1 O1 Zn1 140.1(7) . . ? C1 O2 Zn2 125.9(6) . . ? C5 O3 C8 118.8(7) . . ? C14 O4 Zn1 121.1(5) . 3_675 ? C14 O5 Zn2 146.4(6) . 6_665 ? C15 O6 Zn1 130.2(6) . 3 ? C15 O7 Zn2 133.2(6) . 3 ? C22 O8 C19 115.7(8) . . ? C28 O9 Zn2 132.8(6) . . ? C28 O10 Zn1 133.1(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.619 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.251 #End of Crystallographic Information File