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)
Kengkaj Sukcharoenphon; Kenneth B. Capps; Khalil A. Abboud; Carl D. Hoff; Inorganic Chemistry 40 (2001) 2402–2408; doi:10.1021/ic000722r

data_4319587
_publ_section_title
;
 Synthesis and Structure of W(\h2-mp)2(CO)3 (mp = Monoanion of
 2-Mercaptopyridine) and Its Reactions with 2,2'-Pyridine Disulfide and/or
 NO To Yield W(\h2-mp)4, W(\h2-mp)2(NO)2, and W(\h2-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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0174P)^2^+1.7621P] where P=(Fo^2^+2Fc^2^)/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