#------------------------------------------------------------------------------
#$Date: 2017-10-13 08:09:21 +0200 (vie 13 de oct de 2017) $
#$Revision: 201973 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/13/2201307.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_2201307
loop_
_publ_author_name
'Srinivasan, Bikshandarkoil R. '
'Dhuri, Sunder N.'
'Näther, Christian'
'Bensch, Wolfgang'
_publ_section_title
;
 Ethylenediammonium tetrathiotungstate(VI)
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m622
_journal_page_last               m624
_journal_paper_doi               10.1107/S1600536802017841
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '(C2 H10 N2) [W S4]'
_chemical_formula_moiety         'C2 H10 N2 2+, W S4 2-'
_chemical_formula_sum            'C2 H10 N2 S4 W'
_chemical_formula_weight         374.21
_chemical_name_common            'Ethylenediammonium tetrathiotungstate'
_chemical_name_systematic        ?
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   8.6401(4)
_cell_length_b                   9.3228(5)
_cell_length_c                   11.8281(7)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      8
_cell_volume                     952.75(9)
_computing_cell_refinement       'IPDS Program Package'
_computing_data_collection       'IPDS Program Package (Stoe, 1998)'
_computing_data_reduction        'IPDS Program Package'
_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, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       φ
_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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8270
_diffrn_reflns_theta_full        28.07
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         2.78
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.929
_exptl_absorpt_correction_T_max  0.527
_exptl_absorpt_correction_T_min  0.237
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.435
_refine_diff_density_min         -2.168
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.011(11)
_refine_ls_extinction_coef       0.0101(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         2308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0230
_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/[σ²(Fo²)+(0.036P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0540
_reflns_number_gt                2207
_reflns_number_total             2308
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt6196.cif
_cod_data_source_block           I
_cod_database_code               2201307
_cod_database_fobs_code          2201307
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'
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 0.22871(2) 0.95126(2) 0.395585(17) 0.01863(8) Uani d . 1 . . W
S1 0.00572(16) 1.06275(18) 0.40603(13) 0.0289(3) Uani d . 1 . . S
S2 0.24861(18) 0.84547(16) 0.23137(11) 0.0281(3) Uani d . 1 . . S
S3 0.24657(18) 0.79105(15) 0.53087(12) 0.0281(3) Uani d . 1 . . S
S4 0.41419(18) 1.10907(17) 0.41289(14) 0.0282(3) Uani d . 1 . . S
N1 0.9322(5) 0.9442(7) 0.6633(4) 0.0303(11) Uani d . 1 . . N
H1N1 1.0065 0.9271 0.7137 0.045 Uiso calc R 1 . . H
H2N1 0.9737 0.9816 0.6011 0.045 Uiso calc R 1 . . H
H3N1 0.8845 0.8625 0.6462 0.045 Uiso calc R 1 . . H
C1 0.8188(7) 1.0466(8) 0.7118(5) 0.0317(12) Uani d . 1 . . C
H1A 0.8708 1.1366 0.7278 0.038 Uiso calc R 1 . . H
H1B 0.7803 1.0086 0.7827 0.038 Uiso calc R 1 . . H
C2 0.6847(8) 1.0747(7) 0.6344(6) 0.0354(15) Uani d . 1 . . C
H2A 0.6337 1.1625 0.6579 0.042 Uiso calc R 1 . . H
H2B 0.7234 1.0892 0.5583 0.042 Uiso calc R 1 . . H
N2 0.5706(5) 0.9580(7) 0.6330(4) 0.0283(10) Uani d . 1 . . N
H1N3 0.4932 0.9810 0.5868 0.042 Uiso calc R 1 . . H
H2N3 0.5339 0.9445 0.7025 0.042 Uiso calc R 1 . . H
H3N3 0.6156 0.8778 0.6089 0.042 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 0.01951(11) 0.01741(10) 0.01899(10) 0.00011(7) -0.00033(7) 0.00052(9)
S1 0.0240(6) 0.0345(8) 0.0283(7) 0.0082(5) 0.0018(5) 0.0037(8)
S2 0.0350(8) 0.0283(6) 0.0212(5) 0.0010(6) -0.0001(5) -0.0051(5)
S3 0.0363(8) 0.0237(6) 0.0242(6) -0.0006(6) -0.0038(6) 0.0076(5)
S4 0.0283(7) 0.0278(7) 0.0285(8) -0.0083(5) -0.0024(5) 0.0009(6)
N1 0.023(2) 0.038(3) 0.030(3) -0.001(2) -0.0017(17) 0.002(3)
C1 0.030(3) 0.028(3) 0.037(3) -0.005(3) -0.006(2) -0.006(3)
C2 0.032(3) 0.027(3) 0.047(4) 0.003(2) -0.007(3) 0.009(3)
N2 0.022(2) 0.034(3) 0.029(3) 0.002(2) -0.0026(16) 0.002(3)
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
_geom_angle_publ_flag
S4 W1 S2 109.23(6) y
S4 W1 S1 108.66(7) y
S2 W1 S1 109.46(6) y
S4 W1 S3 109.78(6) y
S2 W1 S3 109.60(6) y
S1 W1 S3 110.08(6) y
C1 N1 H1N1 109.5 n
C1 N1 H2N1 109.5 n
H1N1 N1 H2N1 109.5 n
C1 N1 H3N1 109.5 n
H1N1 N1 H3N1 109.5 n
H2N1 N1 H3N1 109.5 n
N1 C1 C2 112.8(5) y
N1 C1 H1A 109.0 n
C2 C1 H1A 109.0 n
N1 C1 H1B 109.0 n
C2 C1 H1B 109.0 n
H1A C1 H1B 107.8 n
N2 C2 C1 113.3(5) y
N2 C2 H2A 108.9 n
C1 C2 H2A 108.9 n
N2 C2 H2B 108.9 n
C1 C2 H2B 108.9 n
H2A C2 H2B 107.7 n
C2 N2 H1N3 109.5 n
C2 N2 H2N3 109.5 n
H1N3 N2 H2N3 109.5 n
C2 N2 H3N3 109.5 n
H1N3 N2 H3N3 109.5 n
H2N3 N2 H3N3 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 S4 . 2.1851(14) y
W1 S2 . 2.1852(13) y
W1 S1 . 2.1927(14) y
W1 S3 . 2.1943(13) y
N1 C1 . 1.483(8) y
N1 H1N1 . 0.8900 n
N1 H2N1 . 0.8900 n
N1 H3N1 . 0.8900 n
C1 C2 . 1.500(9) y
C1 H1A . 0.9700 n
C1 H1B . 0.9700 n
C2 N2 . 1.468(8) y
C2 H2A . 0.9700 n
C2 H2B . 0.9700 n
N2 H1N3 . 0.8900 n
N2 H2N3 . 0.8900 n
N2 H3N3 . 0.8900 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 S4 2_675 0.89 2.48 3.274(5) 149.4
N1 H1N1 S2 2_675 0.89 3.00 3.478(6) 115.3
N1 H2N1 S1 1_655 0.89 2.44 3.300(6) 161.4
N1 H3N1 S2 4_566 0.89 2.69 3.370(6) 134.1
N1 H3N1 S3 4_566 0.89 2.80 3.558(6) 143.6
N2 H1N3 S4 . 0.89 2.47 3.254(5) 146.5
N2 H1N3 S3 . 0.89 2.85 3.424(6) 123.8
N2 H2N3 S1 2_575 0.89 2.43 3.301(5) 165.5
N2 H3N3 S3 4_566 0.89 2.55 3.385(6) 157.1
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30654665
