A new metalorganic chemical vapor deposition process for MoS<sub>2</sub> with a 1,4-diazabutadienyl stabilized molybdenum precursor and elemental sulfur.
Wree, Jan-Lucas; Ciftyurek, Engin; Zanders, David; Boysen, Nils; Kostka, Aleksander; Rogalla, Detlef; Kasischke, Maren; Ostendorf, Andreas; Schierbaum, Klaus; Devi, Anjana; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13462–13474; doi:10.1039/d0dt02471f

data_7705306
_publ_section_title
;
 A new metalorganic chemical vapor deposition process for MoS<sub>2</sub>
 with a 1,4-diazabutadienyl stabilized molybdenum precursor and elemental
 sulfur.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13462
_journal_page_last               13474
_journal_paper_doi               10.1039/d0dt02471f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C18 H38 Mo N4'
_chemical_formula_sum            'C18 H38 Mo N4'
_chemical_formula_weight         406.46
_chemical_name_common            '[Mo(NtBu)2(tBu2DAD)]'
_chemical_name_systematic
1,4-ditertbutyl-1,4-diazabutadienyl-bis(tertbutylimido)molybdenum(VI)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-04-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-04-17 deposited with the CCDC.	2020-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.033(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3048(2)
_cell_length_b                   10.5005(3)
_cell_length_c                   20.7712(5)
_cell_measurement_reflns_used    15488
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.7550
_cell_measurement_theta_min      4.2140
_cell_volume                     2244.41(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -69.00  25.00   0.50    0.25    --  -47.64  75.00  36.00  188
  2  \w   -119.00 -26.00   0.50    0.25    --  -47.64 -75.00 -91.00  186
  3  \w     26.00 119.00   0.50    0.25    --   47.64  75.00  36.00  186
  4  \w    -24.00  70.00   0.50    0.25    --   47.64 -75.00 -91.00  188
  5  \w   -159.00 -64.00   0.50    1.00    --  -86.25 -75.00 -91.00  190
  6  \w    -95.00 -13.00   0.50    1.00    --  -86.25  75.00  36.00  164
  7  \w     35.00 101.00   0.50    1.00    --  107.75 -75.00 -91.00  132
  8  \w     86.00 156.00   0.50    1.00    --  107.75  75.00  36.00  140
  9  \w    -23.00  27.00   0.50    0.25    --  -47.64  19.00 -30.00  100
 10  \w   -118.00 -74.00   0.50    0.25    --  -47.64-125.00 -30.00   88
 11  \w   -116.00 -76.00   0.50    0.25    --  -47.64-125.00  60.00   80
 12  \w    -48.00 -23.00   0.50    1.00    --  -86.25  45.00   0.00   50
 13  \w    -48.00 -23.00   0.50    1.00    --  -86.25  45.00 120.00   50
 14  \w    -48.00 -15.00   0.50    1.00    --  -86.25  45.00-120.00   66
 15  \w     35.00  67.00   0.50    1.00    --  107.75 -61.00  30.00   64
 16  \w     96.00 176.00   0.50    1.00    --  107.75  45.00   0.00  160
 17  \w    117.00 144.00   0.50    1.00    --  107.75  45.00 -30.00   54
 18  \w     38.00  72.00   0.50    1.00    --  107.75 -61.00 150.00   68
 19  \w     37.00  73.00   0.50    1.00    --  107.75 -61.00   0.00   72
 20  \w     36.00  69.00   0.50    1.00    --  107.75 -61.00-180.00   66
 21  \w     37.00 106.00   0.50    1.00    --  107.75-125.00   0.00  138
 22  \w    116.00 165.00   0.50    1.00    --  107.75  45.00-120.00   98
 23  \w     36.00  62.00   0.50    1.00    --  107.75 -61.00  60.00   52
 24  \w     82.00 108.00   0.50    1.00    --  107.75-125.00-150.00   52
 25  \w     67.00 108.00   0.50    1.00    --  107.75 -77.00  30.00   82
 26  \w     38.00  69.00   0.50    1.00    --  107.75-125.00-150.00   62
 27  \w     41.00  73.00   0.50    1.00    --  107.75 -61.00  90.00   64
 28  \w     36.00  62.00   0.50    1.00    --  107.75 -61.00 120.00   52
 29  \w    150.00 178.00   0.50    1.00    --  107.75  45.00 -30.00   56
 30  \w     47.00  72.00   0.50    1.00    --  107.75 -61.00-150.00   50
 31  \w     39.00 105.00   0.50    1.00    --  107.75 -77.00  90.00  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0746313000
_diffrn_orient_matrix_UB_12      0.0739509000
_diffrn_orient_matrix_UB_13      0.0542845000
_diffrn_orient_matrix_UB_21      0.1296254000
_diffrn_orient_matrix_UB_22      -0.0365571000
_diffrn_orient_matrix_UB_23      -0.0287652000
_diffrn_orient_matrix_UB_31      -0.0063936000
_diffrn_orient_matrix_UB_32      0.1213304000
_diffrn_orient_matrix_UB_33      -0.0417338000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23512
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.761
_diffrn_reflns_theta_min         4.263
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.800
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.374
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.20a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4676
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+1.9937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4423
_reflns_number_total             4676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02471f2.cif
_cod_data_source_block           jlw_modad_010
_cod_depositor_comments          'Adding full bibliography for 7705306.cif.'
_cod_database_code               7705306
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C18 H38 Mo1 N4 '
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.352
_diffrn_oxdiff_ac4_digest_frames
;
01b4f2c5f11023e05ce2992840d79204c50313006bb
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C19 \\sim C3-C19A
 with sigma of 0.02
 C3-C17 \\sim C3-C17A
 with sigma of 0.02
 C3-C18 \\sim C3-C18A
 with sigma of 0.02
3. Others
 Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(1)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
4.a Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C), C5(H5A,
 H5B,H5C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C17A(H17D,H17E,H17F), C19A(H19D,H19E,H19F), C18A(H18D,H18E,H18F)
;
_shelx_res_checksum              41836
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.313
_oxdiff_exptl_absorpt_empirical_full_min 0.814
_publcif_funding_html
;
;