#------------------------------------------------------------------------------ #$Date: 2008-02-04 17:24:24 +0000 (Mon, 04 Feb 2008) $ #$Revision: 87 $ #$URL: svn://www.crystallography.net/cod/cif/2/2204582.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2204582 loop_ _publ_author_name 'Srinivasan, Bikshandarkoil R. ' 'Poisot, Martha' 'N\"ather, Christian' 'Bensch, Wolfgang' _publ_section_title ; Diammonium tetrathiotungstate(VI), (NH~4~)~2~[WS~4~], at 150 K ; _journal_issue 11 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first i136 _journal_page_last i138 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '(N H4)2 [W S4]' _chemical_formula_moiety '2H4 N +, S4 W 2-' _chemical_formula_structural '(N H4)2 [W S4]' _chemical_formula_sum 'H8 N2 S4 W' _chemical_formula_weight 348.17 _chemical_name_common 'diammonium tetrathiotungstate' _chemical_name_systematic ; ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m 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 4 _cell_length_a 9.6054(6) _cell_length_b 6.9863(5) _cell_length_c 12.2557(10) _cell_measurement_reflns_used 7250 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 10 _cell_volume 822.43(10) _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 SHELXTL' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.980 _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 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 7433 _diffrn_reflns_theta_full 27.94 _diffrn_reflns_theta_max 27.94 _diffrn_reflns_theta_min 2.69 _diffrn_standards_decay_% none _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 14.966 _exptl_absorpt_correction_T_max 0.297 _exptl_absorpt_correction_T_min 0.238 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(X-SHAPE; Stoe & Cie, 1998)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 640 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.740 _refine_diff_density_min -1.355 _refine_ls_extinction_coef 0.0029(3) _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 1.097 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 41 _refine_ls_number_reflns 1054 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.097 _refine_ls_R_factor_all 0.0204 _refine_ls_R_factor_gt 0.0183 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0285P)^2^+1.1841P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.0479 _reflns_number_gt 962 _reflns_number_total 1054 _reflns_threshold_expression I>2\s(I) _[local]_cod_original_file wm6034.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, 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 N N 0.0061 0.0033 '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' 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_ _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_type_symbol W1 0.752691(13) 0.7500 0.571606(12) 0.00719(10) Uani d S 1 W S1 0.52833(10) 0.7500 0.61117(8) 0.0151(2) Uani d S 1 S S2 0.78299(12) 0.7500 0.39486(8) 0.0180(2) Uani d S 1 S S3 0.85205(8) 0.49637(11) 0.64144(6) 0.01860(17) Uani d . 1 S N1 0.4537(4) 0.7500 0.3368(3) 0.0144(7) Uani d S 1 N H1N1 0.4820 0.7500 0.2702 0.022 Uiso d SR 1 H H2N1 0.5157 0.7500 0.3873 0.022 Uiso d SR 1 H H3N1 0.4018 0.6509 0.3459 0.022 Uiso d R 1 H N2 0.1658(4) 0.7500 0.6127(3) 0.0168(7) Uani d S 1 N H1N2 0.2335 0.7500 0.6585 0.025 Uiso d SR 1 H H2N2 0.0872 0.7500 0.6463 0.025 Uiso d SR 1 H H3N2 0.1689 0.6497 0.5721 0.025 Uiso d 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 0.00843(13) 0.00605(13) 0.00708(12) 0.000 -0.00001(4) 0.000 S1 0.0111(4) 0.0202(5) 0.0140(5) 0.000 0.0034(3) 0.000 S2 0.0164(5) 0.0294(6) 0.0081(5) 0.000 0.0028(4) 0.000 S3 0.0172(3) 0.0105(3) 0.0282(4) 0.0007(3) -0.0062(3) 0.0082(3) N1 0.0136(16) 0.0153(17) 0.0143(16) 0.000 -0.0026(12) 0.000 N2 0.0156(17) 0.0173(19) 0.0173(17) 0.000 0.0027(13) 0.000 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 S2 . 2.1856(11) y W1 S3 7_575 2.1870(8) y W1 S3 . 2.1870(7) y W1 S1 . 2.2090(10) y N1 H1N1 . 0.8600 n N1 H2N1 . 0.8601 n N1 H3N1 . 0.8600 n N2 H1N2 . 0.8599 n N2 H2N2 . 0.8601 n N2 H3N2 . 0.8600 n 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 W1 S3 . 7_575 109.25(3) y S2 W1 S3 . . 109.25(3) y S3 W1 S3 7_575 . 108.23(4) y S2 W1 S1 . . 110.33(4) y S3 W1 S1 7_575 . 109.87(2) y S3 W1 S1 . . 109.87(2) y H1N1 N1 H2N1 . . 117.6 n H1N1 N1 H3N1 . . 107.9 n H2N1 N1 H3N1 . . 107.9 n H1N2 N2 H2N2 . . 110.6 n H1N2 N2 H3N2 . . 110.6 n H2N2 N2 H3N2 . . 107.9 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 H1N1 S2 6_556 0.86 2.78 3.278(3) 118 N1 H1N1 S3 2_664 0.86 2.83 3.489(3) 135 N1 H1N1 S3 8_765 0.86 2.83 3.489(3) 135 N1 H2N1 S2 . 0.86 2.57 3.242(4) 136 N1 H2N1 S1 . 0.86 2.75 3.439(3) 139 N1 H3N1 S3 5_666 0.86 2.65 3.414(3) 149 N1 H3N1 S1 5_666 0.86 2.93 3.5552(7) 131 N2 H1N2 S1 . 0.86 2.89 3.483(4) 128 N2 H2N2 S3 1_455 0.86 2.87 3.513(3) 133 N2 H2N2 S3 7_475 0.86 2.87 3.513(3) 133 N2 H2N2 S1 6_557 0.86 3.03 3.633(4) 129 N2 H3N2 S3 5_666 0.86 2.82 3.563(3) 146 N2 H3N2 S2 5_666 0.86 2.86 3.5289(6) 136