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_4084330
_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         'C14 H24 Mo N4 O4 S2'
_chemical_formula_sum            'C14 H24 Mo N4 O4 S2'
_chemical_formula_weight         472.43
_chemical_name_systematic
; 
 ? 
;
_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                68.701(11)
_cell_angle_beta                 73.511(13)
_cell_angle_gamma                60.651(12)
_cell_formula_units_Z            2
_cell_length_a                   9.7415(7)
_cell_length_b                   9.8755(8)
_cell_length_c                   13.2893(16)
_cell_measurement_reflns_used    3490
_cell_measurement_temperature    98(2)
_cell_measurement_theta_max      40.2
_cell_measurement_theta_min      1.7
_cell_volume                     1029.4(2)
_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)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      98(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6731
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0300P)^2^+1.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                4483
_reflns_number_total             4696
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500567y_si_002.cif
_cod_data_source_block           '[Mo(CO)4(TMTU)2]'
_cod_depositor_comments
'Adding full bibliography for 4084329--4084332.cif.'
_cod_original_cell_volume        1029.41(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4084330