Synthesis and Characterization of Molybdenum(0) and Tungsten(0) Complexes of Tetramethylthiourea: Single-Source Precursors for MoS2and WS2
Shupp, John P.; Kinne, Adam S.; Arman, Hadi D.; Tonzetich, Zachary J.; Organometallics 33 (2014) 5238–; doi:10.1021/om500567y

data_4084332
_publ_section_title
;
 Synthesis and Characterization of Molybdenum(0) and Tungsten(0) Complexes
 of Tetramethylthiourea: Single-Source Precursors for MoS2and WS2
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5238
_journal_paper_doi               10.1021/om500567y
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C28 H48 N8 O8 S4 W2'
_chemical_formula_sum            'C28 H48 N8 O8 S4 W2'
_chemical_formula_weight         1120.68
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.310(2)
_cell_angle_beta                 94.23(3)
_cell_angle_gamma                119.480(3)
_cell_formula_units_Z            1
_cell_length_a                   9.740(3)
_cell_length_b                   9.873(3)
_cell_length_c                   13.305(4)
_cell_measurement_reflns_used    4517
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      40.2
_cell_measurement_theta_min      1.7
_cell_volume                     1025.4(6)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_diffrn_ambient_temperature      98(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type
;
Saturn724 (2x2 bin mode)
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7382
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.861
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.578
_refine_diff_density_min         -2.375
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0700P)^2^+3.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1176
_reflns_number_gt                3882
_reflns_number_total             4186
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500567y_si_002.cif
_cod_data_source_block           '[W(CO)4(TMTU)2]'
_cod_depositor_comments
'Adding full bibliography for 4084329--4084332.cif.'
_cod_original_cell_volume        1025.4(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4084332