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#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/91/1519124.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_1519124
loop_
_publ_author_name
'Baker, P'
'Hursthouse, Michael B.'
_publ_section_title
;
 C11H6S2N4O3W
;
_journal_name_full               'Crystal Structure Report Archive'
_journal_page_first              1019
_journal_year                    1993
_chemical_formula_sum            'C11 H6 N4 O3 S2 W'
_chemical_formula_weight         490.17
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 111.423(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.896(4)
_cell_length_b                   13.4790(15)
_cell_length_c                   11.6350(7)
_cell_measurement_temperature    293(2)
_cell_volume                     1444.7(6)
_computing_cell_refinement       REFINE
_computing_data_collection       'MADNES (Pflugrath & Messerschmidt, 1989)'
_computing_data_reduction        'ABSURD (Karaulov, 1992)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution
'SIR92 (Altomare, Cascarano, Giacovazzo & Guagliardi, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Delft instruments FAST area detector'
_diffrn_measurement_method
'Intensity measurements as described by Darr, Drake, Hursthouse & Malik (1993)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1082
_diffrn_reflns_av_sigmaI/netI    0.1632
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5452
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    8.298
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            unk
_exptl_crystal_density_diffrn    2.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       unk
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.663
_refine_diff_density_min         -5.455
_refine_diff_density_rms         0.432
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0778
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0825P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2017
_refine_ls_wR_factor_ref         0.2078
_reflns_number_gt                2006
_reflns_number_total             2424
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            eCrystal-1019.cif
_cod_data_source_block           s80
_cod_depositor_comments
;
Citation :
Baker, P and Hursthouse, Michael B. (1993) 
University of Southampton, Crystal Structure Report Archive. 
(doi:10.5258/ecrystals/1019)

http://ecrystals.chem.soton.ac.uk/1019/
;
_cod_original_cell_volume        1444.7(7)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1519124
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.19703(6) 0.18169(4) 0.26748(6) 0.0295(3) Uani 1 1 d . . .
S1 S 0.0316(5) 0.1482(3) 0.0477(4) 0.0432(10) Uani 1 1 d . . .
S2 S 0.2644(5) 0.1265(3) 0.4870(3) 0.0393(9) Uani 1 1 d . . .
O1 O 0.0300(14) 0.3837(9) 0.1913(15) 0.065(4) Uani 1 1 d . . .
O2 O 0.4334(18) 0.3409(11) 0.3974(18) 0.094(6) Uani 1 1 d . . .
O3 O 0.428(2) 0.1670(15) 0.145(3) 0.127(10) Uani 1 1 d . . .
N1 N -0.0184(7) 0.1277(6) 0.2449(6) 0.028(2) Uani 1 1 d G . .
C1 C -0.0783(8) 0.1164(6) 0.1174(6) 0.031(3) Uani 1 1 d G . .
N2 N -0.2204(9) 0.0832(7) 0.0614(6) 0.038(3) Uani 1 1 d G . .
C2 C -0.3025(7) 0.0614(7) 0.1328(8) 0.042(4) Uani 1 1 d G . .
H2 H -0.3976 0.0392 0.0953 0.051 Uiso 1 1 calc R . .
C3 C -0.2426(9) 0.0728(7) 0.2603(8) 0.044(4) Uani 1 1 d G . .
H3 H -0.2976 0.0582 0.3081 0.052 Uiso 1 1 calc R . .
C4 C -0.1005(9) 0.1059(7) 0.3163(5) 0.032(3) Uani 1 1 d G . .
H4 H -0.0605 0.1135 0.4016 0.039 Uiso 1 1 calc R . .
N3 N 0.2565(10) 0.0267(5) 0.3023(7) 0.030(3) Uani 1 1 d G . .
C5 C 0.2852(10) 0.0183(5) 0.4282(7) 0.028(3) Uani 1 1 d G . .
N4 N 0.3265(11) -0.0727(6) 0.4869(6) 0.045(3) Uani 1 1 d G . .
C6 C 0.3389(12) -0.1552(5) 0.4198(9) 0.052(5) Uani 1 1 d G . .
H6 H 0.3665 -0.2160 0.4591 0.063 Uiso 1 1 calc R . .
C7 C 0.3102(12) -0.1467(5) 0.2940(9) 0.044(4) Uani 1 1 d G . .
H7 H 0.3185 -0.2020 0.2491 0.053 Uiso 1 1 calc R . .
C8 C 0.2690(11) -0.0558(6) 0.2353(6) 0.035(3) Uani 1 1 d G . .
H8 H 0.2497 -0.0502 0.1511 0.042 Uiso 1 1 calc R . .
C9 C 0.0917(19) 0.3129(12) 0.2181(19) 0.046(5) Uani 1 1 d . . .
C10 C 0.3448(19) 0.2780(13) 0.3493(18) 0.056(5) Uani 1 1 d . . .
C11 C 0.349(2) 0.1785(13) 0.194(2) 0.061(7) Uani 1 1 d . . .
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'
S S 0.1246 0.1234 '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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
C10 W1 C11 70.8(10) . .
C10 W1 C9 76.8(6) . .
C11 W1 C9 106.8(7) . .
C10 W1 N3 116.8(5) . .
C11 W1 N3 82.1(5) . .
C9 W1 N3 166.0(5) . .
C10 W1 N1 144.9(7) . .
C11 W1 N1 143.5(8) . .
C9 W1 N1 83.0(5) . .
N3 W1 N1 83.5(3) . .
C10 W1 S2 79.9(6) . .
C11 W1 S2 118.2(7) . .
C9 W1 S2 117.7(6) . .
N3 W1 S2 64.6(2) . .
N1 W1 S2 84.7(2) . .
C10 W1 S1 135.7(6) . .
C11 W1 S1 82.6(8) . .
C9 W1 S1 78.0(6) . .
N3 W1 S1 92.8(2) . .
N1 W1 S1 64.7(2) . .
S2 W1 S1 144.36(14) . .
C1 S1 W1 81.2(3) . .
C5 S2 W1 82.4(3) . .
C1 N1 C4 120.0 . .
C1 N1 W1 100.5(4) . .
C4 N1 W1 139.4(4) . .
N2 C1 N1 120.0 . .
N2 C1 S1 126.5(5) . .
N1 C1 S1 113.5(5) . .
C2 N2 C1 120.0 . .
C3 C2 N2 120.0 . .
C3 C2 H2 120.0 . .
N2 C2 H2 120.0 . .
C2 C3 C4 120.0 . .
C2 C3 H3 120.0 . .
C4 C3 H3 120.0 . .
C3 C4 N1 120.0 . .
C3 C4 H4 120.0 . .
N1 C4 H4 120.0 . .
C5 N3 C8 120.0 . .
C5 N3 W1 102.3(4) . .
C8 N3 W1 137.7(4) . .
N4 C5 N3 120.0 . .
N4 C5 S2 129.2(5) . .
N3 C5 S2 110.8(5) . .
C5 N4 C6 120.0 . .
N4 C6 C7 120.0 . .
N4 C6 H6 120.0 . .
C7 C6 H6 120.0 . .
C8 C7 C6 120.0 . .
C8 C7 H7 120.0 . .
C6 C7 H7 120.0 . .
C7 C8 N3 120.0 . .
C7 C8 H8 120.0 . .
N3 C8 H8 120.0 . .
O1 C9 W1 177.8(15) . .
O2 C10 W1 177.4(15) . .
O3 C11 W1 172(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 C10 1.927(18) .
W1 C11 1.988(18) .
W1 C9 2.027(17) .
W1 N3 2.168(6) .
W1 N1 2.175(6) .
W1 S2 2.505(4) .
W1 S1 2.523(4) .
S1 C1 1.633(7) .
S2 C5 1.656(7) .
O1 C9 1.11(2) .
O2 C10 1.20(2) .
O3 C11 1.13(3) .
N1 C1 1.3900 .
N1 C4 1.3900 .
C1 N2 1.3900 .
N2 C2 1.3900 .
C2 C3 1.3900 .
C2 H2 0.9300 .
C3 C4 1.3900 .
C3 H3 0.9300 .
C4 H4 0.9300 .
N3 C5 1.3900 .
N3 C8 1.3900 .
C5 N4 1.3900 .
N4 C6 1.3900 .
C6 C7 1.3900 .
C6 H6 0.9300 .
C7 C8 1.3900 .
C7 H7 0.9300 .
C8 H8 0.9300 .
