Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data__50-010610A _database_code_CSD 188249 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Kondo, Mitsuru' 'Horiba, Tomonori' 'Irie, Yasuhiko' 'Maeda, Kenji' 'Miyazawa, Makoto' 'Naito, Tetsuyoshi' 'Nakamura, Akira' 'Shinagawa, Reiko' 'Uchida, Fumio' 'Utsuni, Shunji' _publ_contact_author_name 'Prof Mitsuru Kondo' _publ_contact_author_address ; Chemistry Shizuoka University 836 Ohya Shizuoka-shi Shizuoka 422-8529 JAPAN ; _publ_contact_author_email 'SCMKOND@IPC.SHIZUOKA.AC.JP' _publ_requested_journal 'Chemical Communications' _publ_section_title ; A new Zn(II) coordination polymer with 4-pyridylthioacetate: assemblies of homo-chiral helices with sulfide sites ; # CHEMICAL DATA _chemical_formula_sum 'C7 H7 N O3 S Zn ' _chemical_formula_moiety 'C7 H7 N O3 S Zn ' _chemical_formula_weight 250.58 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 9.099(5) _cell_length_b 5.098(2) _cell_length_c 10.075(5) _cell_angle_alpha 90 _cell_angle_beta 108.445(6) _cell_angle_gamma 90 _cell_volume 443.4(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1648 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 13.7 _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'cubic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.877 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.975 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 3372 _diffrn_reflns_av_R_equivalents 0.082 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9805 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9805 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1107 _reflns_number_gt 1089 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.0821 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1089 _refine_ls_number_parameters 118 _refine_ls_goodness_of_fit_ref 1.949 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00076|Fo|^2^]' _refine_ls_shift/su_max 0.0003 _refine_diff_density_max 0.84 _refine_diff_density_min -0.91 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack -0.07(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Zn' 'Zn' 0.284 1.430 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Zn(1) Zn 0.52648(5) 0.3999 0.89418(4) 0.0281(1) Uani 1.00 d . . . S(1) S 0.9561(1) 0.3087(3) 0.7077(1) 0.0321(2) Uani 1.00 d . . . O(1) O 0.6922(4) 0.283(1) 0.8215(4) 0.050(1) Uani 1.00 d . . . O(2) O 0.8072(5) 0.046(1) 1.0100(4) 0.049(1) Uani 1.00 d . . . O(3) O 0.4047(4) 0.1664(9) 0.9668(4) 0.0329(7) Uani 1.00 d . . . N(1) N 0.6135(4) 0.040(1) 0.2958(4) 0.0308(8) Uani 1.00 d . . . C(1) C 0.8022(5) 0.143(1) 0.8975(5) 0.0318(9) Uani 1.00 d . . . C(2) C 0.9392(5) 0.097(1) 0.8426(4) 0.0301(9) Uani 1.00 d . . . C(3) C 0.8180(5) 0.194(1) 0.5547(4) 0.0258(9) Uani 1.00 d . . . C(4) C 0.7144(6) -0.018(1) 0.5445(4) 0.032(1) Uani 1.00 d . . . C(5) C 0.6165(5) -0.082(1) 0.4143(4) 0.037(1) Uani 1.00 d . . . C(6) C 0.7131(6) 0.238(1) 0.3061(5) 0.0338(10) Uani 1.00 d . . . C(7) C 0.8150(6) 0.318(1) 0.4310(5) 0.0351(10) Uani 1.00 d . . . H(1) H 0.9313 -0.0773 0.8078 0.0361 Uiso 1.00 calc . . . H(2) H 1.0315 0.1145 0.9197 0.0361 Uiso 1.00 calc . . . H(3) H 0.7130 -0.1131 0.6252 0.0386 Uiso 1.00 calc . . . H(4) H 0.5460 -0.2230 0.4077 0.0443 Uiso 1.00 calc . . . H(5) H 0.7129 0.3273 0.2232 0.0406 Uiso 1.00 calc . . . H(6) H 0.8841 0.4590 0.4332 0.0421 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn(1) 0.0265(2) 0.0363(3) 0.0219(2) 0.0047(2) 0.0084(2) 0.0030(2) S(1) 0.0268(5) 0.0429(6) 0.0258(4) -0.0066(5) 0.0072(3) -0.0073(5) O(1) 0.035(2) 0.086(3) 0.033(2) 0.038(2) 0.016(1) 0.012(2) O(2) 0.041(2) 0.071(3) 0.039(2) 0.003(2) 0.017(1) 0.023(2) O(3) 0.029(1) 0.037(2) 0.035(1) 0.002(1) 0.014(1) 0.003(1) N(1) 0.028(2) 0.039(2) 0.023(1) -0.001(2) 0.005(1) -0.001(2) C(1) 0.025(2) 0.041(2) 0.028(2) -0.002(2) 0.005(1) -0.006(2) C(2) 0.025(2) 0.036(2) 0.025(2) 0.005(2) 0.003(1) -0.005(1) C(3) 0.023(2) 0.033(2) 0.022(1) 0.000(2) 0.008(1) -0.007(1) C(4) 0.039(2) 0.034(2) 0.023(2) -0.013(2) 0.008(1) -0.006(2) C(5) 0.039(2) 0.044(3) 0.025(1) -0.021(2) 0.007(2) -0.003(2) C(6) 0.035(2) 0.042(2) 0.023(2) -0.011(2) 0.008(1) 0.001(2) C(7) 0.034(2) 0.041(2) 0.028(2) -0.016(2) 0.007(1) 0.001(2) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution QTAN _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn(1) O(1) 1.966(5) . . yes Zn(1) O(3) 1.922(6) . . yes Zn(1) O(3) 1.909(5) . 2_657 yes Zn(1) N(1) 2.063(5) . 2_656 yes S(1) C(2) 1.780(7) . . yes S(1) C(3) 1.751(6) . . yes O(1) C(1) 1.269(9) . . yes O(2) C(1) 1.225(9) . . yes N(1) C(5) 1.341(9) . . yes N(1) C(6) 1.338(10) . . yes C(1) C(2) 1.533(9) . . yes C(3) C(4) 1.419(10) . . yes C(3) C(7) 1.390(9) . . yes C(4) C(5) 1.372(8) . . yes C(6) C(7) 1.367(9) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Zn(1) O(3) 123.8(3) . . . yes O(1) Zn(1) O(3) 112.2(3) . . 2_657 yes O(1) Zn(1) N(1) 94.7(2) . . 2_656 yes O(3) Zn(1) O(3) 104.8(1) . . 2_657 yes O(3) Zn(1) N(1) 107.9(2) . . 2_656 yes O(3) Zn(1) N(1) 113.4(3) 2_657 . 2_656 yes C(2) S(1) C(3) 105.0(3) . . . yes Zn(1) O(1) C(1) 119.9(5) . . . yes Zn(1) O(3) Zn(1) 128.7(3) . . 2_647 yes Zn(1) N(1) C(5) 119.8(5) 2_646 . . yes Zn(1) N(1) C(6) 122.5(4) 2_646 . . yes C(5) N(1) C(6) 117.4(5) . . . yes O(1) C(1) O(2) 125.2(7) . . . yes O(1) C(1) C(2) 116.4(6) . . . yes O(2) C(1) C(2) 118.4(6) . . . yes S(1) C(2) C(1) 117.4(5) . . . yes S(1) C(3) C(4) 126.4(5) . . . yes S(1) C(3) C(7) 116.3(5) . . . yes C(4) C(3) C(7) 117.2(5) . . . yes C(3) C(4) C(5) 117.9(6) . . . yes N(1) C(5) C(4) 124.3(7) . . . yes N(1) C(6) C(7) 122.8(6) . . . yes C(3) C(7) C(6) 120.4(7) . . . yes #------------------------------------------------------------------------------ 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 Zn(1) O(1) C(1) O(2) 8(1) . . . . yes Zn(1) O(1) C(1) C(2) -170.5(5) . . . . yes Zn(1) O(3) Zn(1) O(1) 164.6(3) . . 2_647 2_647 yes Zn(1) O(3) Zn(1) O(3) -58.6(4) . . 2_647 2_647 yes Zn(1) O(3) Zn(1) O(1) 51.6(4) . 2_657 2_657 2_657 yes Zn(1) O(3) Zn(1) O(3) -78.7(5) . 2_657 2_657 1_565 yes Zn(1) N(1) C(5) C(4) 174.4(7) . 2_656 2_656 2_656 yes Zn(1) N(1) C(6) C(7) -174.5(6) . 2_656 2_656 2_656 yes S(1) C(2) C(1) O(1) 16.5(9) . . . . yes S(1) C(2) C(1) O(2) -162.9(7) . . . . yes S(1) C(3) C(4) C(5) -178.6(6) . . . . yes S(1) C(3) C(7) C(6) 178.7(6) . . . . yes O(1) Zn(1) N(1) C(5) 34.6(7) . . 2_656 2_656 yes O(1) Zn(1) N(1) C(6) -151.2(6) . . 2_656 2_656 yes O(3) Zn(1) O(1) C(1) -54.9(8) . . . . yes O(3) Zn(1) O(3) Zn(1) -58.6(4) . . 2_657 2_657 yes O(3) Zn(1) N(1) C(5) -93.2(6) . . 2_656 2_656 yes O(3) Zn(1) N(1) C(6) 81.0(6) . . 2_656 2_656 yes O(3) Zn(1) O(1) C(1) 72.3(8) . 2_647 2_647 2_647 yes N(1) Zn(1) O(1) C(1) -170.1(7) . 2_646 2_646 2_646 yes N(1) C(5) C(4) C(3) 0(1) . . . . yes N(1) C(6) C(7) C(3) 0(1) . . . . yes C(1) C(2) S(1) C(3) -77.2(6) . . . . yes C(2) S(1) C(3) C(4) 1.1(7) . . . . yes C(2) S(1) C(3) C(7) -175.9(6) . . . . yes C(4) C(3) C(7) C(6) 1(1) . . . . yes C(4) C(5) N(1) C(6) 0(1) . . . . yes C(5) N(1) C(6) C(7) 0(1) . . . . yes C(5) C(4) C(3) C(7) -1(1) . . . . yes C(5) C(4) C(3) C(7) -1(1) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Zn(1) Zn(1) 3.4536(8) . 2_647 ? S(1) O(2) 3.211(6) . 2_757 ? O(2) O(3) 2.793(9) . 2_647 ? O(2) C(2) 3.254(10) . 2_747 ? O(2) C(6) 3.495(9) . 1_556 ? O(3) O(3) 3.036(5) . 2_647 ? O(3) N(1) 3.320(7) . 1_556 ? O(3) C(6) 3.407(9) . 2_646 ? C(5) C(7) 3.53(1) . 1_545 ? #------------------------------------------------------------------------------