Synthesis, structure, DFT calculations, and full vibrational analysis of the prototypical thioformaldehyde complex mer-[W(CO)3(Me2PC2H4PMe2)(η2-SCH2)]
Wolfdieter A. Schenk; Birgit Vedder; Matthias Klüglein; Damien Moigno; Wolfgang Kiefer; J. Chem. Soc., Dalton Trans.  (2002) 3123–3128; doi:10.1039/b203195g

data_7011707
_publ_section_title
;
 Synthesis, structure, DFT calculations, and full vibrational analysis
 of the prototypical thioformaldehyde complex
 mer-[W(CO)3(Me2PC2H4PMe2)(\h2-SCH2)]
;
_journal_issue                   16
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              3123
_journal_page_last               3128
_journal_paper_doi               10.1039/b203195g
_journal_year                    2002
_chemical_formula_sum            'C10 H18 O3 P2 S W'
_chemical_formula_weight         464.09
_chemical_melting_point          74
_chemical_name_systematic
; 
[Tricarbonyl-bis(dimethylphosphino)ethane-thioformaldehyde-tungsten] 
;
_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                 90.4830(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1843(5)
_cell_length_b                   12.4238(7)
_cell_length_c                   13.6206(7)
_cell_measurement_reflns_used    6336
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.082
_cell_measurement_theta_min      2.685
_cell_volume                     1554.11(15)
_computing_cell_refinement       'Smart 5.620'
_computing_data_collection       'Smart 5.622'
_computing_data_reduction        'Saint Plus'
_computing_publication_material  shelxl-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART Apex with D8-Goniometer'
_diffrn_measurement_method       'omega 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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25623
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0.2
_diffrn_standards_interval_time  5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.767
_exptl_absorpt_correction_T_max  0.5106
_exptl_absorpt_correction_T_min  0.5106
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.304
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0189
_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^)+(0.0222P)^2^+1.5144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0449
_reflns_number_gt                3257
_reflns_number_total             3414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203195g.txt
_cod_data_source_block           biwo2b
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7011707