#------------------------------------------------------------------------------ #$Date: 2025-08-19 11:43:10 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301803 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/23/2202334.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_2202334 loop_ _publ_author_name 'Srinivasan, Bikshandarkoil R. ' 'Dhuri, Sunder N. ' 'N\"ather, Christian' 'Bensch, Wolfgang' _publ_section_title ; 1,4-Dimethylpiperazinium tetrathiotungstate(VI) ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m681 _journal_page_last m683 _journal_paper_doi 10.1107/S1600536803016040 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '(C6 H16 N2) [W1 S4]' _chemical_formula_moiety 'C6 H16 N2 2+, S4 W 2-' _chemical_formula_sum 'C6 H16 N2 S4 W' _chemical_formula_weight 428.30 _chemical_name_systematic ; 1,4-dimethylpiperazinium tetrathiotungstate(VI) ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _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 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 13.3792(11) _cell_length_b 12.6369(7) _cell_length_c 14.9381(9) _cell_measurement_reflns_used 8000 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 23 _cell_measurement_theta_min 15 _cell_volume 2525.6(3) _computing_cell_refinement IPDS _computing_data_collection 'IPDS (Stoe & Cie, 1998)' _computing_data_reduction IPDS _computing_molecular_graphics 'XP in SHELXTL (Bruker, 1998)' _computing_publication_material 'CIFTAB in SHELXL97' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.962 _diffrn_measured_fraction_theta_max 0.962 _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method \f _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 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 23034 _diffrn_reflns_theta_full 28.03 _diffrn_reflns_theta_max 28.03 _diffrn_reflns_theta_min 2.60 _diffrn_standards_decay_% none _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 9.771 _exptl_absorpt_correction_T_max 0.555 _exptl_absorpt_correction_T_min 0.360 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(X-SHAPE and X-RED; Stoe & Cie, 1998)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1632 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _refine_diff_density_max 1.658 _refine_diff_density_min -1.389 _refine_ls_extinction_coef 0.00187(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 119 _refine_ls_number_reflns 2946 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.013 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0246 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0453P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.0668 _reflns_number_gt 2398 _reflns_number_total 2946 _reflns_threshold_expression I>2s(I) _cod_data_source_file bt6303.cif _cod_data_source_block I _cod_database_code 2202334 _cod_database_fobs_code 2202334 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' loop_ _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 _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol W1 0.248391(6) 0.345321(12) 0.628045(7) 0.01946(8) Uani d . 1 . . W S1 0.10187(5) 0.28939(7) 0.67238(5) 0.03026(18) Uani d . 1 . . S S2 0.27210(6) 0.29591(8) 0.48747(5) 0.03188(19) Uani d . 1 . . S S3 0.36779(6) 0.28653(8) 0.71377(6) 0.0422(2) Uani d . 1 . . S S4 0.24917(5) 0.51921(10) 0.63317(6) 0.0315(2) Uani d . 1 . . S N1 0.40873(17) 0.5130(2) 0.44850(16) 0.0259(5) Uani d . 1 . . N H1 0.3655 0.4801 0.4864 0.031 Uiso calc R 1 . . H C1 0.4875(2) 0.4348(3) 0.4221(2) 0.0301(7) Uani d . 1 . . C H1A 0.5332 0.4676 0.3801 0.036 Uiso calc R 1 . . H H1B 0.4563 0.3750 0.3924 0.036 Uiso calc R 1 . . H C2 0.5454(2) 0.3958(3) 0.5027(2) 0.0298(7) Uani d . 1 . . C H2A 0.5010 0.3577 0.5426 0.036 Uiso calc R 1 . . H H2B 0.5975 0.3476 0.4834 0.036 Uiso calc R 1 . . H C3 0.3513(3) 0.5492(4) 0.3687(2) 0.0462(10) Uani d . 1 . . C H3A 0.3226 0.4891 0.3389 0.069 Uiso calc R 1 . . H H3B 0.3953 0.5857 0.3283 0.069 Uiso calc R 1 . . H H3C 0.2990 0.5963 0.3874 0.069 Uiso calc R 1 . . H N11 0.49326(17) 0.5178(2) -0.09605(16) 0.0242(5) Uani d . 1 . . N H11 0.5495 0.4829 -0.1135 0.029 Uiso calc R 1 . . H C11 0.5237(2) 0.6048(3) -0.0332(2) 0.0271(7) Uani d . 1 . . C H11A 0.4652 0.6450 -0.0156 0.032 Uiso calc R 1 . . H H11B 0.5695 0.6524 -0.0634 0.032 Uiso calc R 1 . . H C12 0.5736(2) 0.5597(3) 0.0492(2) 0.0274(6) Uani d . 1 . . C H12A 0.6352 0.5247 0.0320 0.033 Uiso calc R 1 . . H H12B 0.5904 0.6168 0.0899 0.033 Uiso calc R 1 . . H C13 0.4438(3) 0.5618(3) -0.1780(2) 0.0386(8) Uani d . 1 . . C H13A 0.4253 0.5048 -0.2172 0.058 Uiso calc R 1 . . H H13B 0.4893 0.6082 -0.2084 0.058 Uiso calc R 1 . . H H13C 0.3851 0.6005 -0.1609 0.058 Uiso calc R 1 . . H 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 W1 0.01603(10) 0.02096(13) 0.02140(11) 0.00036(3) -0.00050(3) -0.00104(4) S1 0.0255(3) 0.0339(5) 0.0315(4) -0.0083(3) 0.0074(3) -0.0023(3) S2 0.0328(3) 0.0385(5) 0.0243(4) -0.0032(3) 0.0054(3) -0.0064(3) S3 0.0378(4) 0.0442(6) 0.0446(5) 0.0144(4) -0.0204(4) -0.0072(4) S4 0.0327(5) 0.0186(6) 0.0431(5) -0.0018(3) 0.0004(3) -0.0012(3) N1 0.0238(11) 0.0298(16) 0.0241(12) -0.0004(10) 0.0030(9) 0.0050(10) C1 0.0262(14) 0.037(2) 0.0277(16) 0.0034(13) 0.0030(12) -0.0074(13) C2 0.0298(15) 0.023(2) 0.0365(18) 0.0048(11) 0.0044(13) 0.0008(12) C3 0.042(2) 0.061(3) 0.035(2) 0.0072(17) -0.0080(14) 0.0092(16) N11 0.0244(11) 0.0261(15) 0.0221(12) -0.0003(10) 0.0027(9) 0.0019(10) C11 0.0323(16) 0.0216(19) 0.0273(16) -0.0058(11) 0.0018(12) 0.0013(11) C12 0.0270(14) 0.0278(19) 0.0274(16) -0.0078(12) -0.0001(11) -0.0009(13) C13 0.0475(19) 0.045(2) 0.0234(16) 0.0015(16) -0.0049(14) 0.0062(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' W W -0.8490 6.8722 '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 S3 W1 S1 . . 111.67(4) y S3 W1 S4 . . 108.48(3) y S1 W1 S4 . . 108.46(3) y S3 W1 S2 . . 110.88(4) y S1 W1 S2 . . 108.94(3) y S4 W1 S2 . . 108.32(3) y C3 N1 C2 . 5_666 111.4(3) y C3 N1 C1 . . 110.8(3) y C2 N1 C1 5_666 . 110.4(2) y C3 N1 H1 . . 108.1 n C2 N1 H1 5_666 . 108.1 n C1 N1 H1 . . 108.1 n N1 C1 C2 . . 111.5(2) y N1 C1 H1A . . 109.3 n C2 C1 H1A . . 109.3 n N1 C1 H1B . . 109.3 n C2 C1 H1B . . 109.3 n H1A C1 H1B . . 108.0 n N1 C2 C1 5_666 . 110.3(3) y N1 C2 H2A 5_666 . 109.6 n C1 C2 H2A . . 109.6 n N1 C2 H2B 5_666 . 109.6 n C1 C2 H2B . . 109.6 n H2A C2 H2B . . 108.1 n N1 C3 H3A . . 109.5 n N1 C3 H3B . . 109.5 n H3A C3 H3B . . 109.5 n N1 C3 H3C . . 109.5 n H3A C3 H3C . . 109.5 n H3B C3 H3C . . 109.5 n C13 N11 C12 . 5_665 111.1(2) y C13 N11 C11 . . 111.1(3) y C12 N11 C11 5_665 . 110.4(2) y C13 N11 H11 . . 108.1 n C12 N11 H11 5_665 . 108.1 n C11 N11 H11 . . 108.1 n N11 C11 C12 . . 110.7(3) y N11 C11 H11A . . 109.5 n C12 C11 H11A . . 109.5 n N11 C11 H11B . . 109.5 n C12 C11 H11B . . 109.5 n H11A C11 H11B . . 108.1 n N11 C12 C11 5_665 . 111.3(2) y N11 C12 H12A 5_665 . 109.4 n C11 C12 H12A . . 109.4 n N11 C12 H12B 5_665 . 109.4 n C11 C12 H12B . . 109.4 n H12A C12 H12B . . 108.0 n N11 C13 H13A . . 109.5 n N11 C13 H13B . . 109.5 n H13A C13 H13B . . 109.5 n N11 C13 H13C . . 109.5 n H13A C13 H13C . . 109.5 n H13B C13 H13C . . 109.5 n 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 W1 S3 . 2.1781(8) y W1 S1 . 2.1866(7) y W1 S4 . 2.1988(12) y W1 S2 . 2.2136(8) y N1 C3 . 1.491(4) y N1 C2 5_666 1.495(4) y N1 C1 . 1.497(4) y N1 H1 . 0.91 n C1 C2 . 1.514(5) y C1 H1A . 0.97 n C1 H1B . 0.97 n C2 N1 5_666 1.495(4) y C2 H2A . 0.97 n C2 H2B . 0.97 n C3 H3A . 0.96 n C3 H3B . 0.96 n C3 H3C . 0.96 n N11 C13 . 1.499(4) y N11 C12 5_665 1.500(4) y N11 C11 . 1.502(4) y N11 H11 . 0.91 n C11 C12 . 1.512(5) y C11 H11A . 0.97 n C11 H11B . 0.97 n C12 N11 5_665 1.500(4) y C12 H12A . 0.97 n C12 H12B . 0.97 n C13 H13A . 0.96 n C13 H13B . 0.96 n C13 H13C . 0.96 n 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 N1 H1 S2 . 0.91 2.64 3.347(3) 135 N1 H1 S4 . 0.91 2.73 3.489(2) 141 N11 H11 S1 6_656 0.91 2.69 3.427(3) 139 N11 H11 S4 6_656 0.91 2.73 3.468(2) 139 loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139065975