#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:03:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179275 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/95/4319587.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_4319587
loop_
_publ_author_name
'Kengkaj Sukcharoenphon'
'Kenneth B. Capps'
'Khalil A. Abboud'
'Carl D. Hoff'
_publ_section_title
;
 Synthesis and Structure of W(η2-mp)2(CO)3 (mp = Monoanion of
 2-Mercaptopyridine) and Its Reactions with 2,2'-Pyridine Disulfide and/or
 NO To Yield W(η2-mp)4, W(η2-mp)2(NO)2, and W(η2-mp)3(NO)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2402
_journal_page_last               2408
_journal_paper_doi               10.1021/ic000722r
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C16 H14 Cl2 N4 O S3 W'
_chemical_formula_weight         629.24
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           62
_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                   15.0210(6)
_cell_length_b                   15.0846(6)
_cell_length_c                   8.9312(4)
_cell_measurement_temperature    173(2)
_cell_volume                     2023.68(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-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    0.0189
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            14558
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    6.297
_exptl_absorpt_correction_T_max  0.524
_exptl_absorpt_correction_T_min  0.322
_exptl_absorpt_correction_type   Emirical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.065
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plates
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00466(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0177
_refine_ls_R_factor_gt           0.0156
_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)+(0.0174P)²+1.7621P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0372
_refine_ls_wR_factor_ref         0.0379
_reflns_number_gt                2238
_reflns_number_total             2413
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000722r_3.cif
_cod_data_source_block           hof9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2023.7(1)
_cod_database_code               4319587
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_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
W W 0.182848(8) 0.2500 0.463219(13) 0.01992(6) Uani 1 2 d S . .
S1 S 0.26222(5) 0.2500 0.21906(9) 0.02579(16) Uani 1 2 d S . .
N1 N 0.09373(19) 0.2500 0.2656(3) 0.0292(6) Uani 1 2 d S . .
C1 C 0.1528(2) 0.2500 0.1510(4) 0.0292(7) Uani 1 2 d S . .
C2 C 0.1244(3) 0.2500 0.0026(4) 0.0412(9) Uani 1 2 d S . .
H2A H 0.1659 0.2500 -0.0776 0.049 Uiso 1 2 calc SR . .
C3 C 0.0340(3) 0.2500 -0.0241(4) 0.0601(14) Uani 1 2 d S . .
H3A H 0.0126 0.2500 -0.1241 0.072 Uiso 1 2 calc SR . .
C4 C -0.0258(3) 0.2500 0.0939(5) 0.0622(15) Uani 1 2 d S . .
H4A H -0.0881 0.2500 0.0753 0.075 Uiso 1 2 calc SR . .
C5 C 0.0060(2) 0.2500 0.2386(4) 0.0426(10) Uani 1 2 d S . .
H5A H -0.0347 0.2500 0.3201 0.051 Uiso 1 2 calc SR . .
S1' S 0.07289(4) 0.34765(4) 0.59824(7) 0.02797(13) Uani 1 1 d . . .
N1' N 0.19723(13) 0.39492(13) 0.4273(2) 0.0260(4) Uani 1 1 d . . .
C1' C 0.13136(16) 0.43160(15) 0.5094(3) 0.0252(5) Uani 1 1 d . . .
C2' C 0.11790(18) 0.52310(16) 0.5147(3) 0.0313(5) Uani 1 1 d . . .
H2'A H 0.0708 0.5477 0.5722 0.038 Uiso 1 1 calc R . .
C3' C 0.1747(2) 0.57679(18) 0.4344(3) 0.0397(6) Uani 1 1 d . . .
H3'A H 0.1665 0.6392 0.4344 0.048 Uiso 1 1 calc R . .
C4' C 0.2435(2) 0.53923(18) 0.3539(3) 0.0456(7) Uani 1 1 d . . .
H4'A H 0.2838 0.5758 0.2999 0.055 Uiso 1 1 calc R . .
C5' C 0.25346(19) 0.44842(17) 0.3523(3) 0.0382(6) Uani 1 1 d . . .
H5'A H 0.3011 0.4230 0.2971 0.046 Uiso 1 1 calc R . .
O2 O 0.32568(17) 0.2500 0.6970(3) 0.0366(6) Uani 1 2 d S . .
N2 N 0.26785(18) 0.2500 0.6019(3) 0.0245(5) Uani 1 2 d S . .
Cl1 Cl 0.0325(4) 0.4627(4) 0.1391(3) 0.0764(14) Uani 0.504(12) 1 d P . 1
C6 C -0.0185(10) 0.4458(9) -0.0476(12) 0.048(4) Uani 0.252(6) 1 d P . 1
H6A H 0.0199 0.4057 -0.1070 0.058 Uiso 0.252(6) 1 calc PR . 1
H6B H -0.0770 0.4164 -0.0349 0.058 Uiso 0.252(6) 1 calc PR . 1
Cl1' Cl 0.0668(4) 0.5052(5) 0.1183(5) 0.0887(19) Uani 0.496(12) 1 d P . 2
C6' C 0.0379(8) 0.4957(10) -0.0614(14) 0.049(4) Uani 0.248(6) 1 d P . 2
H6'A H 0.0676 0.5448 -0.1152 0.059 Uiso 0.248(6) 1 calc PR . 2
H6'B H 0.0653 0.4401 -0.0983 0.059 Uiso 0.248(6) 1 calc PR . 2
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
N2 W N1 171.30(11) . . ?
N2 W N1' 91.77(5) . . ?
N1 W N1' 86.76(5) . . ?
N2 W N1' 91.77(5) . 7_565 ?
N1 W N1' 86.76(5) . 7_565 ?
N1' W N1' 159.92(10) . 7_565 ?
N2 W S1 105.46(9) . . ?
N1 W S1 65.85(7) . . ?
N1' W S1 80.00(5) . . ?
N1' W S1 80.00(5) 7_565 . ?
N2 W S1' 97.89(7) . . ?
N1 W S1' 89.15(6) . . ?
N1' W S1' 63.73(5) . . ?
N1' W S1' 135.11(5) 7_565 . ?
S1 W S1' 137.240(16) . . ?
N2 W S1' 97.89(7) . 7_565 ?
N1 W S1' 89.15(6) . 7_565 ?
N1' W S1' 135.11(5) . 7_565 ?
N1' W S1' 63.73(5) 7_565 7_565 ?
S1 W S1' 137.240(17) . 7_565 ?
S1' W S1' 71.53(3) . 7_565 ?
C1 S1 W 81.62(11) . . ?
C5 N1 C1 120.6(3) . . ?
C5 N1 W 137.5(2) . . ?
C1 N1 W 101.9(2) . . ?
N1 C1 C2 121.3(3) . . ?
N1 C1 S1 110.6(2) . . ?
C2 C1 S1 128.1(3) . . ?
C3 C2 C1 117.8(4) . . ?
C2 C3 C4 120.5(4) . . ?
C5 C4 C3 119.3(4) . . ?
N1 C5 C4 120.6(4) . . ?
C1' S1' W 82.87(8) . . ?
C5' N1' C1' 119.0(2) . . ?
C5' N1' W 136.32(17) . . ?
C1' N1' W 104.69(15) . . ?
N1' C1' C2' 122.0(2) . . ?
N1' C1' S1' 108.71(17) . . ?
C2' C1' S1' 129.3(2) . . ?
C3' C2' C1' 118.3(2) . . ?
C2' C3' C4' 119.6(3) . . ?
C5' C4' C3' 119.6(3) . . ?
N1' C5' C4' 121.5(3) . . ?
O2 N2 W 179.8(3) . . ?
C6 Cl1 C6 67.0(8) 5_565 . ?
Cl1 C6 Cl1 113.0(8) 5_565 . ?
C6' Cl1' C6' 57.0(7) 5_565 . ?
Cl1' C6' Cl1' 123.0(7) 5_565 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W N2 1.779(3) . ?
W N1 2.215(3) . ?
W N1' 2.220(2) . ?
W N1' 2.220(2) 7_565 ?
W S1 2.4853(8) . ?
W S1' 2.5204(6) . ?
W S1' 2.5204(6) 7_565 ?
S1 C1 1.753(4) . ?
N1 C5 1.340(4) . ?
N1 C1 1.354(4) . ?
C1 C2 1.393(5) . ?
C2 C3 1.378(6) . ?
C3 C4 1.385(6) . ?
C4 C5 1.378(5) . ?
S1' C1' 1.733(2) . ?
N1' C5' 1.346(3) . ?
N1' C1' 1.350(3) . ?
C1' C2' 1.396(3) . ?
C2' C3' 1.377(4) . ?
C3' C4' 1.382(4) . ?
C4' C5' 1.378(4) . ?
O2 N2 1.215(4) . ?
Cl1 C6 1.618(13) 5_565 ?
Cl1 C6 1.853(12) . ?
C6 Cl1 1.618(13) 5_565 ?
Cl1' C6' 1.653(14) 5_565 ?
Cl1' C6' 1.669(13) . ?
C6' Cl1' 1.653(14) 5_565 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 W S1 C1 180.0 . . . . ?
N1 W S1 C1 0.0 . . . . ?
N1' W S1 C1 -90.93(5) . . . . ?
N1' W S1 C1 90.93(5) 7_565 . . . ?
S1' W S1 C1 -59.42(3) . . . . ?
S1' W S1 C1 59.42(3) 7_565 . . . ?
N2 W N1 C5 180.0 . . . . ?
N1' W N1 C5 -99.51(5) . . . . ?
N1' W N1 C5 99.51(5) 7_565 . . . ?
S1 W N1 C5 180.0 . . . . ?
S1' W N1 C5 -35.770(13) . . . . ?
S1' W N1 C5 35.770(13) 7_565 . . . ?
N2 W N1 C1 0.0 . . . . ?
N1' W N1 C1 80.49(5) . . . . ?
N1' W N1 C1 -80.49(5) 7_565 . . . ?
S1 W N1 C1 0.0 . . . . ?
S1' W N1 C1 144.230(13) . . . . ?
S1' W N1 C1 -144.230(13) 7_565 . . . ?
C5 N1 C1 C2 0.0 . . . . ?
W N1 C1 C2 180.0 . . . . ?
C5 N1 C1 S1 180.0 . . . . ?
W N1 C1 S1 0.0 . . . . ?
W S1 C1 N1 0.0 . . . . ?
W S1 C1 C2 180.0 . . . . ?
N1 C1 C2 C3 0.0 . . . . ?
S1 C1 C2 C3 180.0 . . . . ?
C1 C2 C3 C4 0.0 . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C1 N1 C5 C4 0.0 . . . . ?
W N1 C5 C4 180.0 . . . . ?
C3 C4 C5 N1 0.0 . . . . ?
N2 W S1' C1' 88.36(9) . . . . ?
N1 W S1' C1' -86.52(9) . . . . ?
N1' W S1' C1' 0.29(10) . . . . ?
N1' W S1' C1' -171.07(10) 7_565 . . . ?
S1 W S1' C1' -34.74(9) . . . . ?
S1' W S1' C1' -175.91(8) 7_565 . . . ?
N2 W N1' C5' 79.4(3) . . . . ?
N1 W N1' C5' -92.0(3) . . . . ?
N1' W N1' C5' -20.6(5) 7_565 . . . ?
S1 W N1' C5' -26.0(2) . . . . ?
S1' W N1' C5' 177.4(3) . . . . ?
S1' W N1' C5' -177.5(2) 7_565 . . . ?
N2 W N1' C1' -98.31(17) . . . . ?
N1 W N1' C1' 90.27(16) . . . . ?
N1' W N1' C1' 161.6(2) 7_565 . . . ?
S1 W N1' C1' 156.30(15) . . . . ?
S1' W N1' C1' -0.39(13) . . . . ?
S1' W N1' C1' 4.73(18) 7_565 . . . ?
C5' N1' C1' C2' 2.3(4) . . . . ?
W N1' C1' C2' -179.45(19) . . . . ?
C5' N1' C1' S1' -177.69(19) . . . . ?
W N1' C1' S1' 0.53(18) . . . . ?
W S1' C1' N1' -0.46(15) . . . . ?
W S1' C1' C2' 179.5(2) . . . . ?
N1' C1' C2' C3' -0.7(4) . . . . ?
S1' C1' C2' C3' 179.3(2) . . . . ?
C1' C2' C3' C4' -1.1(4) . . . . ?
C2' C3' C4' C5' 1.4(5) . . . . ?
C1' N1' C5' C4' -2.1(4) . . . . ?
W N1' C5' C4' -179.6(2) . . . . ?
C3' C4' C5' N1' 0.3(5) . . . . ?
N1 W N2 O2 180.0(2) . . . . ?
N1' W N2 O2 99.9(2) . . . . ?
N1' W N2 O2 -99.9(2) 7_565 . . . ?
S1 W N2 O2 180.0(2) . . . . ?
S1' W N2 O2 36.2(2) . . . . ?
S1' W N2 O2 -36.2(2) 7_565 . . . ?
C6 Cl1 C6 Cl1 0.0 5_565 . . 5_565 ?
C6' Cl1' C6' Cl1' 0.0 5_565 . . 5_565 ?
