#------------------------------------------------------------------------------
#$Date: 2017-10-13 03:48:21 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201957 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/01/58/2015820.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_2015820
loop_
_publ_author_name
'Srinivasan, Bikshandarkoil R. '
'Naik, Ashish R. '
'Näther, Christian'
'Bensch, Wolfgang'
_publ_section_title
;
 Competing hydrogen-bond acceptors in ethylenediammonium
 oxotrithiotungstate(VI)
;
_journal_coeditor_code           AV3050
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m81
_journal_page_last               m84
_journal_paper_doi               10.1107/S0108270106056393
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C2 H10 N2) [W O S3]'
_chemical_formula_moiety         'C2 H10 N2 +, O S3 W -'
_chemical_formula_sum            'C2 H10 N2 O S3 W'
_chemical_formula_weight         358.15
_chemical_name_common            'ethylenediammonium oxotrithiotungstate(VI)'
_chemical_name_systematic
;
ethylenediammonium oxotrithiotungstate(VI)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.631(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8191(14)
_cell_length_b                   10.7923(18)
_cell_length_c                   9.3793(14)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      20.1
_cell_volume                     892.7(2)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1998)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1998)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'CIFTAB in SHELXTL (Bruker, 1998)'
_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 AED-II four-circle'
_diffrn_measurement_method       ω/θ
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3022
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.88
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  'every 120 min'
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    13.576
_exptl_absorpt_correction_T_max  0.135
_exptl_absorpt_correction_T_min  0.091
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.791
_refine_diff_density_min         -2.128
_refine_ls_extinction_coef       0.0020(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         2602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0261
_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)+(0.0334P)²+2.4809P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0697
_reflns_number_gt                2052
_reflns_number_total             2602
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            av3050.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2015820
_cod_database_fobs_code          2015820
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_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
W W1 0.23427(2) 0.62410(2) 0.188568(19) 0.02179(8) Uani d . 1
S S1 0.03782(16) 0.61605(15) 0.33097(16) 0.0339(3) Uani d . 1
S S2 0.23135(19) 0.46562(14) 0.04054(15) 0.0339(3) Uani d . 1
S S3 0.2303(2) 0.79721(14) 0.06900(17) 0.0378(3) Uani d . 1
O O1 0.4038(4) 0.6187(4) 0.2927(5) 0.0327(8) Uani d . 1
N N1 0.5718(5) 0.8387(5) 0.2825(5) 0.0292(9) Uani d . 1
H H1N1 0.6153 0.8627 0.3641 0.044 Uiso calc R 1
H H2N1 0.5082 0.7765 0.2994 0.044 Uiso calc R 1
H H3N1 0.5209 0.9019 0.2443 0.044 Uiso calc R 1
N N2 0.9214(6) 0.9070(5) 0.2668(6) 0.0383(12) Uani d . 1
H H1N2 0.8755 0.9298 0.3466 0.057 Uiso calc R 1
H H2N2 0.9897 0.9639 0.2432 0.057 Uiso calc R 1
H H3N2 0.9675 0.8345 0.2805 0.057 Uiso calc R 1
C C1 0.6906(7) 0.7969(6) 0.1820(6) 0.0340(12) Uani d . 1
H H1A 0.6423 0.7718 0.0932 0.041 Uiso calc R 1
H H1B 0.7414 0.7249 0.2220 0.041 Uiso calc R 1
C C2 0.8076(7) 0.8948(7) 0.1506(7) 0.0413(15) Uani d . 1
H H2A 0.8587 0.8739 0.0628 0.050 Uiso calc R 1
H H2B 0.7571 0.9738 0.1366 0.050 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
W1 0.02061(10) 0.02227(11) 0.02250(11) -0.00107(8) -0.00015(6) -0.00098(8)
S1 0.0291(6) 0.0346(7) 0.0383(7) -0.0028(6) 0.0095(5) -0.0052(6)
S2 0.0447(8) 0.0270(6) 0.0300(6) -0.0008(6) 0.0050(6) -0.0065(5)
S3 0.0516(9) 0.0268(7) 0.0349(7) -0.0049(6) -0.0023(6) 0.0070(6)
O1 0.0265(17) 0.0297(19) 0.042(2) -0.0019(17) -0.0037(16) 0.0007(18)
N1 0.027(2) 0.028(2) 0.033(2) -0.0030(17) -0.0015(18) -0.0030(19)
N2 0.030(2) 0.038(3) 0.047(3) -0.003(2) 0.004(2) -0.004(2)
C1 0.033(3) 0.036(3) 0.033(3) -0.003(2) 0.002(2) -0.007(2)
C2 0.034(3) 0.053(4) 0.037(3) 0.001(3) -0.001(2) 0.012(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'
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'
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
O1 W1 S3 108.63(14) y
O1 W1 S1 109.15(14) y
S3 W1 S1 109.75(7) y
O1 W1 S2 108.95(15) y
S3 W1 S2 109.96(6) y
S1 W1 S2 110.36(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
C2 N2 H1N2 109.5 n
C2 N2 H2N2 109.5 n
H1N2 N2 H2N2 109.5 n
C2 N2 H3N2 109.5 n
H1N2 N2 H3N2 109.5 n
H2N2 N2 H3N2 109.5 n
N1 C1 C2 113.5(5) y
N1 C1 H1A 108.9 n
C2 C1 H1A 108.9 n
N1 C1 H1B 108.9 n
C2 C1 H1B 108.9 n
H1A C1 H1B 107.7 n
N2 C2 C1 112.2(5) y
N2 C2 H2A 109.2 n
C1 C2 H2A 109.2 n
N2 C2 H2B 109.2 n
C1 C2 H2B 109.2 n
H2A C2 H2B 107.9 n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
W1 O1 1.778(4) y
W1 S3 2.1791(15) y
W1 S1 2.2010(14) y
W1 S2 2.2029(14) y
N1 C1 1.487(7) y
N1 H1N1 0.8900 n
N1 H2N1 0.8900 n
N1 H3N1 0.8900 n
N2 C2 1.479(8) y
N2 H1N2 0.8900 n
N2 H2N2 0.8900 n
N2 H3N2 0.8900 n
C1 C2 1.508(9) y
C1 H1A 0.9700 n
C1 H1B 0.9700 n
C2 H2A 0.9700 n
C2 H2B 0.9700 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 4_676 0.89 2.68 3.496(5) 153
N1 H1N1 S3 4_676 0.89 2.77 3.353(5) 125
N1 H2N1 O1 . 0.89 1.94 2.801(6) 163
N1 H3N1 S1 2 0.89 2.47 3.317(5) 159
N2 H1N2 S2 4_676 0.89 2.50 3.375(6) 168
N2 H2N2 O1 2_655 0.89 1.95 2.816(7) 165
N2 H3N2 S1 1_655 0.89 2.48 3.356(6) 167
C1 H1A S1 4_675 0.97 2.88 3.666(6) 138
C2 H2A O1 4_675 0.97 2.57 3.474(8) 155
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30654053
