Reaction of .NO Thiolate and Thiol Complexes: Elimination of PhSNO from W(phen)(CO)2(SPh)2, CO from W(phen)(CO)2((-S)2Arene), and HNO from W(phen)(CO)3(RSH)
Kenneth B. Capps; Andreas Bauer; Khalil A. Abboud; Carl D. Hoff; Inorganic Chemistry 38 (1999) 6212–6217; doi:10.1021/ic990830h

data_4322567
_publ_section_title
;
 Reaction of .NO Thiolate and Thiol Complexes: Elimination of PhSNO from
 W(phen)(CO)2(SPh)2, CO from W(phen)(CO)2((-S)2Arene), and HNO from
 W(phen)(CO)3(RSH)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6212
_journal_page_last               6217
_journal_paper_doi               10.1021/ic990830h
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C20 H13 N3 O3 S W'
_chemical_formula_weight         559.24
_chemical_name_systematic
; 
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c 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            8
_cell_length_a                   14.2099(7)
_cell_length_b                   13.8261(7)
_cell_length_c                   18.9295(9)
_cell_measurement_temperature    173(2)
_cell_volume                     3719.0(3)
_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  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25366
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    6.351
_exptl_absorpt_correction_T_max  0.530
_exptl_absorpt_correction_T_min  0.372
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.998
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00047(2)
_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   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0164
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0113P)^2^+3.8791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0358
_refine_ls_wR_factor_ref         0.0381
_reflns_number_gt                3617
_reflns_number_total             4266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990830h_1.cif
_cod_data_source_block           hof2
_cod_database_code               4322567