Molybdenum and Tungsten Complexes of Sulfene (Thioformaldehyde S,S-Dioxide)1
Wolfdieter A. Schenk; Katja Nielsen; Nicolai I. Burzlaff; Michael Hagel; Inorganic Chemistry 41 (2002) 1079–1085; doi:10.1021/ic010963e

data_4317640
_publ_contact_author
;
              Prof. Dr. Wolfdieter A. Schenk
              Institut f\"ur Anorganische Chemie
              Universit\"at W\"urzburg
              Am Hubland
              D-97074 W\"urzburg
              Germany
;
_publ_contact_author_email       wolfdieter.schenk@mail.uni-wuerzburg.de
_publ_contact_author_fax         '+49 931 8884605'
_publ_contact_author_phone       '+49 931 8885259'
_publ_section_title
;
 Molybdenum and Tungsten Complexes of Sulfene (Thioformaldehyde
 S,S-Dioxide)1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1079
_journal_page_last               1085
_journal_paper_doi               10.1021/ic010963e
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C29 H24 O5 P2 S W'
_chemical_formula_weight         730.33
_chemical_name_common            '[W(dppm)(CO)3(SO2CH2)]'
_chemical_name_systematic
;
  ?
;
_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                 95.58(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.719(2)
_cell_length_b                   17.392(4)
_cell_length_c                   13.441(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     2726.5(10)
_computing_cell_refinement       'SDP (ENRAF NONIUS)'
_computing_data_collection       'ENRAF NONIUS CAD4'
_computing_data_reduction        'SDP (ENRAF NONIUS)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'ENRAF-NONIUS CAD4'
_diffrn_measurement_method       Omega-Theta-scans
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4274
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        -8.9
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.469
_exptl_absorpt_correction_T_max  0.5085
_exptl_absorpt_correction_T_min  0.4012
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.357
_refine_diff_density_min         -2.995
_refine_diff_density_rms         0.229
_refine_ls_extinction_coef       0.0008(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   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4274
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0519
_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/[\s^2^(Fo^2^)+(0.0754P)^2^+29.1872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1504
_reflns_number_gt                3271
_reflns_number_total             4274
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010963e_3.cif
_cod_data_source_block           Nielsen-1-10a
_cod_original_cell_volume        2726.6(9)
_cod_database_code               4317640