#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2015321.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_2015321 loop_ _publ_author_name 'Song, Yan-Wei' 'Yu, Zhan' 'Zhang, Qian-Feng' _publ_section_title ; \g-Modification of poly[(N,N-diethyldithiocarbamato)silver(I)] ; _journal_coeditor_code OB3001 _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m214 _journal_page_last m216 _journal_volume 62 _journal_year 2006 _chemical_formula_iupac '[Ag3 (C5 H10 N S2)3]' _chemical_formula_moiety 'C15 H30 Ag3 N3 S6' _chemical_formula_sum 'C15 H30 Ag3 N3 S6' _chemical_formula_weight 768.45 _chemical_name_systematic ; catena-poly[[trisilver(I)-di-\m~3~-N,N-diethyldithiocarbamato- 3'\kS:1\kS':2\kS;1\kS:2\kS':3\kS- \m~4~-N,N-diethyldithiocarbamato- 2\kS:3\k^2^S,S':1'\kS'] ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _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 105.30(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 18.138(4) _cell_length_b 9.5890(19) _cell_length_c 14.245(3) _cell_measurement_reflns_used 2887 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 18.26 _cell_measurement_theta_min 2.33 _cell_volume 2389.8(9) _computing_cell_refinement 'SAINT-Plus (Bruker, 1998)' _computing_data_collection 'SMART (Bruker, 1998)' _computing_data_reduction SAINT-Plus _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997b)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997a)' _diffrn_ambient_temperature 153(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _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 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 7241 _diffrn_reflns_theta_full 28.28 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_min 2.33 _exptl_absorpt_coefficient_mu 2.966 _exptl_absorpt_correction_T_max 0.586 _exptl_absorpt_correction_T_min 0.457 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 2.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1512 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _refine_diff_density_max 1.592 _refine_diff_density_min -0.971 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 124 _refine_ls_number_reflns 2853 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.086 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0335 _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^)+(0.0369P)^2^+2.307P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.0793 _reflns_number_gt 2506 _reflns_number_total 2853 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ob3001.cif _[local]_cod_data_source_block III _[local]_cod_cif_authors_sg_H-M C2/c _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 2389.8(8) _cod_database_code 2015321 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 0.519534(16) 0.37249(3) 0.55071(2) 0.02157(10) Uani d . 1 Ag Ag2 0.5000 0.56129(4) 0.7500 0.01967(11) Uani d S 1 S S1 0.57677(5) 0.31786(9) 0.40397(6) 0.01522(18) Uani d . 1 S S2 0.57616(5) 0.32543(9) 0.72706(6) 0.01755(18) Uani d . 1 S S3 0.37699(5) 0.41359(9) 0.48830(6) 0.01747(19) Uani d . 1 N N1 0.70878(16) 0.4503(3) 0.4185(2) 0.0137(6) Uani d . 1 N N2 0.5000 0.0960(4) 0.7500 0.0150(8) Uani d S 1 C C1 0.64259(19) 0.4536(3) 0.4414(2) 0.0149(7) Uani d . 1 C C2 0.5000 0.2339(5) 0.7500 0.0157(9) Uani d S 1 C C11 0.76313(19) 0.5670(4) 0.4412(2) 0.0169(7) Uani d . 1 H H11A 0.7351 0.6536 0.4396 0.020 Uiso calc R 1 H H11B 0.7911 0.5724 0.3920 0.020 Uiso calc R 1 C C12 0.81906(19) 0.5506(4) 0.5403(3) 0.0207(8) Uani d . 1 H H12A 0.8542 0.6274 0.5520 0.031 Uiso calc R 1 H H12B 0.8468 0.4649 0.5422 0.031 Uiso calc R 1 H H12C 0.7917 0.5490 0.5895 0.031 Uiso calc R 1 C C13 0.7341(2) 0.3304(4) 0.3700(3) 0.0192(7) Uani d . 1 H H13A 0.7102 0.2462 0.3856 0.023 Uiso calc R 1 H H13B 0.7890 0.3198 0.3948 0.023 Uiso calc R 1 C C14 0.7144(2) 0.3475(5) 0.2611(3) 0.0289(9) Uani d . 1 H H14A 0.7320 0.2675 0.2326 0.043 Uiso calc R 1 H H14B 0.7387 0.4298 0.2452 0.043 Uiso calc R 1 H H14C 0.6601 0.3560 0.2360 0.043 Uiso calc R 1 C C21 0.56207(19) 0.0118(4) 0.7296(2) 0.0169(7) Uani d . 1 H H21A 0.5671 -0.0748 0.7659 0.020 Uiso calc R 1 H H21B 0.6100 0.0622 0.7507 0.020 Uiso calc R 1 C C22 0.5461(2) -0.0203(4) 0.6220(3) 0.0213(8) Uani d . 1 H H22A 0.5882 -0.0713 0.6101 0.032 Uiso calc R 1 H H22B 0.5394 0.0653 0.5858 0.032 Uiso calc R 1 H H22C 0.5004 -0.0752 0.6019 0.032 Uiso calc R 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 0.02415(17) 0.02126(16) 0.02314(17) 0.00380(11) 0.01298(12) 0.00766(11) Ag2 0.0214(2) 0.01563(19) 0.0194(2) 0.000 0.00092(14) 0.000 S1 0.0172(4) 0.0133(4) 0.0156(4) -0.0013(3) 0.0050(3) -0.0007(3) S2 0.0187(4) 0.0163(4) 0.0196(4) -0.0015(3) 0.0085(3) 0.0004(3) S3 0.0189(4) 0.0175(4) 0.0177(4) -0.0013(3) 0.0077(3) -0.0057(3) N1 0.0170(14) 0.0124(14) 0.0132(14) -0.0005(11) 0.0066(11) -0.0003(11) N2 0.018(2) 0.019(2) 0.0096(19) 0.000 0.0063(15) 0.000 C1 0.0158(16) 0.0144(16) 0.0131(15) 0.0008(13) 0.0016(12) 0.0023(13) C2 0.017(2) 0.018(2) 0.012(2) 0.000 0.0025(17) 0.000 C11 0.0177(17) 0.0162(17) 0.0182(17) -0.0040(13) 0.0070(13) 0.0029(14) C12 0.0177(18) 0.0196(18) 0.0250(19) -0.0028(14) 0.0058(14) 0.0006(15) C13 0.0200(18) 0.0192(18) 0.0205(18) 0.0045(14) 0.0092(14) -0.0017(15) C14 0.033(2) 0.038(2) 0.0184(19) 0.0036(17) 0.0111(16) -0.0082(17) C21 0.0185(17) 0.0153(16) 0.0190(18) 0.0013(13) 0.0084(13) 0.0009(14) C22 0.0245(18) 0.0232(19) 0.0197(18) -0.0036(15) 0.0118(14) -0.0058(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' 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_ _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 S2 Ag1 S3 . . 119.54(4) yes S2 Ag1 S1 . . 128.56(3) yes S3 Ag1 S1 . . 109.49(4) yes S2 Ag1 Ag1 . 5_666 130.65(3) ? S3 Ag1 Ag1 . 5_666 65.92(3) ? S1 Ag1 Ag1 . 5_666 82.20(2) ? S2 Ag1 S3 . 5_666 101.75(3) yes S3 Ag1 S3 . 5_666 118.03(2) yes S1 Ag1 S3 . 5_666 65.19(3) yes Ag1 Ag1 S3 5_666 5_666 52.11(2) ? S1 Ag2 S1 6_566 5_666 125.84(4) yes S1 Ag2 S2 6_566 2_656 117.10(3) ? S1 Ag2 S2 5_666 2_656 107.63(3) ? S1 Ag2 S2 6_566 . 107.63(3) yes S1 Ag2 S2 5_666 . 117.10(3) yes S2 Ag2 S2 2_656 . 67.15(4) yes C1 S1 Ag2 . 5_666 95.63(11) ? C1 S1 Ag1 . . 89.44(12) ? Ag2 S1 Ag1 5_666 . 110.76(3) ? C2 S2 Ag1 . . 98.30(5) ? C2 S2 Ag2 . . 86.75(15) ? Ag1 S2 Ag2 . . 83.28(3) ? C1 S3 Ag1 5_666 . 105.08(12) ? C1 S3 Ag1 5_666 5_666 80.35(12) ? Ag1 S3 Ag1 . 5_666 61.97(2) ? C1 N1 C11 . . 121.8(3) ? C1 N1 C13 . . 123.2(3) ? C11 N1 C13 . . 115.0(3) ? C2 N2 C21 . 2_656 123.19(19) ? C2 N2 C21 . . 123.2(2) ? C21 N2 C21 2_656 . 113.6(4) ? N1 C1 S3 . 5_666 120.1(3) ? N1 C1 S1 . . 119.8(3) ? S3 C1 S1 5_666 . 120.0(2) ? N2 C2 S2 . . 120.32(14) ? N2 C2 S2 . 2_656 120.32(14) ? S2 C2 S2 . 2_656 119.4(3) ? N1 C11 C12 . . 111.8(3) ? N1 C11 H11A . . 109.3 ? C12 C11 H11A . . 109.3 ? N1 C11 H11B . . 109.3 ? C12 C11 H11B . . 109.3 ? H11A C11 H11B . . 107.9 ? C11 C12 H12A . . 109.5 ? C11 C12 H12B . . 109.5 ? H12A C12 H12B . . 109.5 ? C11 C12 H12C . . 109.5 ? H12A C12 H12C . . 109.5 ? H12B C12 H12C . . 109.5 ? N1 C13 C14 . . 112.3(3) ? N1 C13 H13A . . 109.1 ? C14 C13 H13A . . 109.1 ? N1 C13 H13B . . 109.1 ? C14 C13 H13B . . 109.1 ? H13A C13 H13B . . 107.9 ? C13 C14 H14A . . 109.5 ? C13 C14 H14B . . 109.5 ? H14A C14 H14B . . 109.5 ? C13 C14 H14C . . 109.5 ? H14A C14 H14C . . 109.5 ? H14B C14 H14C . . 109.5 ? N2 C21 C22 . . 111.0(3) ? N2 C21 H21A . . 109.4 ? C22 C21 H21A . . 109.4 ? N2 C21 H21B . . 109.4 ? C22 C21 H21B . . 109.4 ? H21A C21 H21B . . 108.0 ? C21 C22 H22A . . 109.5 ? C21 C22 H22B . . 109.5 ? H22A C22 H22B . . 109.5 ? C21 C22 H22C . . 109.5 ? H22A C22 H22C . . 109.5 ? H22B C22 H22C . . 109.5 ? 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 S2 . 2.4915(11) yes Ag1 S3 . 2.5333(11) yes Ag1 S1 . 2.6205(11) yes Ag1 Ag1 5_666 2.8336(7) yes Ag1 S3 5_666 2.9308(10) yes Ag2 S1 6_566 2.5457(11) ? Ag2 S1 5_666 2.5457(11) yes Ag2 S2 2_656 2.7145(10) ? Ag2 S2 . 2.7145(10) yes S1 C1 . 1.751(3) ? S1 Ag2 5_666 2.5457(11) ? S2 C2 . 1.739(3) ? S3 C1 5_666 1.714(4) ? S3 Ag1 5_666 2.9308(10) ? N1 C1 . 1.325(4) ? N1 C11 . 1.470(4) ? N1 C13 . 1.476(4) ? N2 C2 . 1.322(6) ? N2 C21 2_656 1.476(4) ? N2 C21 . 1.476(4) ? C1 S3 5_666 1.714(4) ? C2 S2 2_656 1.739(3) ? C11 C12 . 1.513(5) ? C11 H11A . 0.9700 ? C11 H11B . 0.9700 ? C12 H12A . 0.9600 ? C12 H12B . 0.9600 ? C12 H12C . 0.9600 ? C13 C14 . 1.507(5) ? C13 H13A . 0.9700 ? C13 H13B . 0.9700 ? C14 H14A . 0.9600 ? C14 H14B . 0.9600 ? C14 H14C . 0.9600 ? C21 C22 . 1.514(5) ? C21 H21A . 0.9700 ? C21 H21B . 0.9700 ? C22 H22A . 0.9600 ? C22 H22B . 0.9600 ? C22 H22C . 0.9600 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion S2 Ag1 S1 C1 . . -72.66(11) S3 Ag1 S1 C1 . . 125.33(11) Ag1 Ag1 S1 C1 5_666 . 64.37(11) S3 Ag1 S1 C1 5_666 . 12.66(11) S2 Ag1 S1 Ag2 . 5_666 -168.48(3) S3 Ag1 S1 Ag2 . 5_666 29.52(4) Ag1 Ag1 S1 Ag2 5_666 5_666 -31.45(3) S3 Ag1 S1 Ag2 5_666 5_666 -83.16(4) S3 Ag1 S2 C2 . . 33.91(15) S1 Ag1 S2 C2 . . -126.53(15) Ag1 Ag1 S2 C2 5_666 . 116.36(15) S3 Ag1 S2 C2 5_666 . 165.95(14) S3 Ag1 S2 Ag2 . . -51.79(4) S1 Ag1 S2 Ag2 . . 147.77(3) Ag1 Ag1 S2 Ag2 5_666 . 30.65(4) S3 Ag1 S2 Ag2 5_666 . 80.24(3) S1 Ag2 S2 C2 6_566 . 112.63(4) S1 Ag2 S2 C2 5_666 . -98.84(4) S2 Ag2 S2 C2 2_656 . 0.0 S1 Ag2 S2 Ag1 6_566 . -148.61(3) S1 Ag2 S2 Ag1 5_666 . -0.08(4) S2 Ag2 S2 Ag1 2_656 . 98.76(4) S2 Ag1 S3 C1 . 5_666 54.42(13) S1 Ag1 S3 C1 . 5_666 -141.70(12) Ag1 Ag1 S3 C1 5_666 5_666 -70.11(12) S3 Ag1 S3 C1 5_666 5_666 -70.11(12) S2 Ag1 S3 Ag1 . 5_666 124.54(3) S1 Ag1 S3 Ag1 . 5_666 -71.58(3) S3 Ag1 S3 Ag1 5_666 5_666 0.0 C11 N1 C1 S3 . 5_666 -7.8(4) C13 N1 C1 S3 . 5_666 171.4(2) C11 N1 C1 S1 . . 174.9(2) C13 N1 C1 S1 . . -5.9(4) Ag2 S1 C1 N1 5_666 . -95.0(3) Ag1 S1 C1 N1 . . 154.2(3) Ag2 S1 C1 S3 5_666 5_666 87.69(19) Ag1 S1 C1 S3 . 5_666 -23.12(19) C21 N2 C2 S2 2_656 . 178.98(16) C21 N2 C2 S2 . . -1.02(16) C21 N2 C2 S2 2_656 2_656 -1.02(16) C21 N2 C2 S2 . 2_656 178.98(16) Ag1 S2 C2 N2 . . 97.28(4) Ag2 S2 C2 N2 . . 180.0 Ag1 S2 C2 S2 . 2_656 -82.72(4) Ag2 S2 C2 S2 . 2_656 0.0000(10) C1 N1 C11 C12 . . 90.4(4) C13 N1 C11 C12 . . -88.9(4) C1 N1 C13 C14 . . 94.4(4) C11 N1 C13 C14 . . -86.4(4) C2 N2 C21 C22 . . -90.5(3) C21 N2 C21 C22 2_656 . 89.5(3)