#------------------------------------------------------------------------------ #$Date: 2009-11-16 03:43:51 +0200 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2211221.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2211221 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _publ_author_name 'Zhang, Hongming' 'Gondi, Sudershan R.' 'Son, David Y.' _publ_section_title ; Poly[\m~3~-1,3-dithiolane-2-methanol-\k^3^S:S:S'-\m-nitrato-silver(I)] ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m3086 _journal_page_last m3088 _journal_volume 62 _journal_year 2006 _chemical_formula_iupac '[Ag (N O3) (C4 H8 O S2)]' _chemical_formula_moiety 'C4 H8 Ag N O4 S2' _chemical_formula_sum 'C4 H8 Ag N O4 S2' _chemical_formula_weight 306.10 _chemical_name_systematic ; Poly[\m~3~-1,3-dithiolane-2-methanol-\k~3~S:S:S'-\m-nitrato-silver(I)] ; _symmetry_cell_setting monoclinic _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 104.5970(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.4659(7) _cell_length_b 6.6555(5) _cell_length_c 13.9767(10) _cell_measurement_reflns_used 3583 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 27.74 _cell_measurement_theta_min 2.98 _cell_volume 852.11(11) _computing_cell_refinement 'SAINT (Bruker, 1997)' _computing_data_collection 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_molecular_graphics 'SHELXTL (Bruker, 1997)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 296(2) _diffrn_detector_area_resol_mean 83.33 _diffrn_measured_fraction_theta_full 0.965 _diffrn_measured_fraction_theta_max 0.965 _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_av_sigmaI/netI 0.017 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 7522 _diffrn_reflns_theta_full 28.25 _diffrn_reflns_theta_max 28.25 _diffrn_reflns_theta_min 2.35 _exptl_absorpt_coefficient_mu 2.828 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_correction_T_min 0.415 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 1997)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_description thin-plate _exptl_crystal_F_000 600 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.451 _refine_diff_density_min -0.518 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 110 _refine_ls_number_reflns 2039 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.036 _refine_ls_R_factor_gt 0.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+1.5745P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.077 _refine_ls_wR_factor_ref 0.079 _reflns_number_gt 1870 _reflns_number_total 2039 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file wk2028.cif 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy Ag Ag1 0.63194(3) 0.20899(4) 0.33123(2) 0.04569(12) Uani d . 1 C C1 0.5138(4) 0.7103(5) 0.2533(2) 0.0349(7) Uani d . 1 H H1 0.5111 0.6328 0.1933 0.042 Uiso calc R 1 S S2 0.68952(9) 0.84145(12) 0.28994(6) 0.03357(18) Uani d . 1 C C3 0.7608(4) 0.7233(5) 0.4093(3) 0.0382(7) Uani d . 1 H H3A 0.8171 0.6049 0.4023 0.046 Uiso calc R 1 H H3B 0.8238 0.8159 0.4542 0.046 Uiso calc R 1 C C4 0.6323(4) 0.6654(5) 0.4492(2) 0.0366(7) Uani d . 1 H H4A 0.5878 0.7844 0.4692 0.044 Uiso calc R 1 H H4B 0.6637 0.5782 0.5062 0.044 Uiso calc R 1 S S5 0.50275(9) 0.53613(11) 0.35123(6) 0.03304(18) Uani d . 1 C C6 0.3864(4) 0.8592(6) 0.2308(3) 0.0545(10) Uani d . 1 H H6A 0.3921 0.9401 0.1742 0.065 Uiso calc R 1 H H6B 0.2955 0.7846 0.2131 0.065 Uiso calc R 1 O O7 0.3841(3) 0.9871(4) 0.3100(3) 0.0612(8) Uani d . 1 H H7 0.3474 0.9282 0.3494 0.092 Uiso calc R 1 N N1 0.8387(4) 0.1954(4) 0.5396(2) 0.0463(7) Uani d . 1 O O1 0.7037(3) 0.1576(5) 0.5224(2) 0.0633(8) Uani d . 1 O O2 0.8892(4) 0.2376(6) 0.4687(3) 0.0711(9) Uani d . 1 O O3 0.9156(4) 0.1854(5) 0.6244(2) 0.0711(10) Uani d . 1 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 Ag1 0.0566(2) 0.02957(16) 0.04904(19) 0.00501(11) 0.00982(13) -0.00315(11) C1 0.0409(17) 0.0282(15) 0.0339(16) -0.0053(13) 0.0062(13) 0.0006(12) S2 0.0378(4) 0.0266(4) 0.0403(4) -0.0035(3) 0.0172(3) 0.0002(3) C3 0.0371(17) 0.0326(16) 0.0422(18) -0.0001(13) 0.0046(14) 0.0000(14) C4 0.0466(18) 0.0331(16) 0.0320(15) -0.0004(14) 0.0134(14) -0.0006(13) S5 0.0348(4) 0.0247(3) 0.0418(4) -0.0023(3) 0.0138(3) 0.0025(3) C6 0.0407(19) 0.0370(19) 0.074(3) -0.0019(16) -0.0070(18) 0.0151(19) O7 0.0517(17) 0.0358(14) 0.100(2) 0.0099(12) 0.0257(17) 0.0076(15) N1 0.0554(19) 0.0318(15) 0.0447(17) 0.0061(13) -0.0007(15) -0.0023(13) O1 0.0561(18) 0.072(2) 0.0610(19) 0.0048(16) 0.0126(15) -0.0060(16) O2 0.064(2) 0.092(3) 0.0556(19) -0.0078(18) 0.0105(16) 0.0148(18) O3 0.087(2) 0.069(2) 0.0434(16) 0.0067(18) -0.0097(16) -0.0001(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ag1 S5 . 2.5468(8) y Ag1 S2 1_545 2.6024(9) y Ag1 O1 . 2.609(3) y Ag1 O2 . 2.702(4) y Ag1 S2 2_645 2.8185(8) y Ag1 O3 4_565 3.171(3) y C1 C6 . 1.531(5) ? C1 S5 . 1.816(3) ? C1 S2 . 1.833(3) ? C1 H1 . 0.9800 ? S2 C3 . 1.814(4) ? S2 Ag1 1_565 2.6024(8) ? S2 Ag1 2_655 2.8185(8) ? C3 C4 . 1.510(5) ? C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? C4 S5 . 1.809(3) ? C4 H4A . 0.9700 ? C4 H4B . 0.9700 ? C6 O7 . 1.401(6) ? C6 H6A . 0.9700 ? C6 H6B . 0.9700 ? O7 H7 . 0.8200 ? N1 O3 . 1.227(5) ? N1 O2 . 1.236(5) ? N1 O1 . 1.265(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S5 Ag1 S2 . 1_545 163.97(3) y S5 Ag1 O1 . . 90.45(8) y S2 Ag1 O1 1_545 . 95.10(8) y S5 Ag1 O2 . . 103.49(9) y S2 Ag1 O2 1_545 . 91.29(9) y O1 Ag1 O2 . . 47.57(10) y S5 Ag1 S2 . 2_645 100.12(3) y S2 Ag1 S2 1_545 2_645 88.279(17) y O1 Ag1 S2 . 2_645 128.02(7) y O2 Ag1 S2 . 2_645 80.56(8) y C6 C1 S5 . . 112.1(3) ? C6 C1 S2 . . 111.2(2) ? S5 C1 S2 . . 108.30(17) ? C6 C1 H1 . . 108.4 ? S5 C1 H1 . . 108.4 ? S2 C1 H1 . . 108.4 ? C3 S2 C1 . . 98.70(16) ? C3 S2 Ag1 . 1_565 104.69(12) ? C1 S2 Ag1 . 1_565 106.47(11) ? C3 S2 Ag1 . 2_655 106.08(12) ? C1 S2 Ag1 . 2_655 108.81(11) ? Ag1 S2 Ag1 1_565 2_655 128.17(3) ? C4 C3 S2 . . 107.6(2) ? C4 C3 H3A . . 110.2 ? S2 C3 H3A . . 110.2 ? C4 C3 H3B . . 110.2 ? S2 C3 H3B . . 110.2 ? H3A C3 H3B . . 108.5 ? C3 C4 S5 . . 107.3(2) ? C3 C4 H4A . . 110.3 ? S5 C4 H4A . . 110.3 ? C3 C4 H4B . . 110.3 ? S5 C4 H4B . . 110.3 ? H4A C4 H4B . . 108.5 ? C4 S5 C1 . . 96.32(15) ? C4 S5 Ag1 . . 103.72(12) ? C1 S5 Ag1 . . 110.03(11) ? O7 C6 C1 . . 113.5(3) ? O7 C6 H6A . . 108.9 ? C1 C6 H6A . . 108.9 ? O7 C6 H6B . . 108.9 ? C1 C6 H6B . . 108.9 ? H6A C6 H6B . . 107.7 ? C6 O7 H7 . . 109.5 ? O3 N1 O2 . . 122.1(4) ? O3 N1 O1 . . 119.9(4) ? O2 N1 O1 . . 118.0(3) ? N1 O1 Ag1 . . 99.1(2) ? N1 O2 Ag1 . . 95.3(2) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O7 H7 O1 3_666 0.82 2.05 2.843(5) 162.1