Synthesis and properties of MoCl<sub>4</sub> complexes with thio- and seleno-ethers and their use for chemical vapour deposition of MoSe<sub>2</sub> and MoS<sub>2</sub> films.
Chang, Yao-Pang; Hector, Andrew L.; Levason, William; Reid, Gillian; Whittam, Joshua; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2406–2414; doi:10.1039/c7dt04352j

data_7045436
_publ_section_title
;
 Synthesis and properties of MoCl<sub>4</sub> complexes with thio- and
 seleno-ethers and their use for chemical vapour deposition of
 MoSe<sub>2</sub> and MoS<sub>2</sub> films.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2406
_journal_page_last               2414
_journal_paper_doi               10.1039/c7dt04352j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C4 H10 Cl4 Mo S2'
_chemical_formula_sum            'C4 H10 Cl4 Mo S2'
_chemical_formula_weight         359.98
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-20 deposited with the CCDC.
2017-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.913(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.1386(6)
_cell_length_b                   11.1622(6)
_cell_length_c                   7.8033(7)
_cell_measurement_reflns_used    3685
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.3640
_cell_measurement_theta_min      2.8700
_cell_volume                     559.27(9)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5766
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.902
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    2.442
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.138
_exptl_crystal_description       plate
_exptl_crystal_F_000             352
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2'
_exptl_crystal_size_max          0.041
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.171
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.163
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   -0.13(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         2142
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0858P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1223
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1903
_reflns_number_total             2142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04352j2.cif
_cod_data_source_block           2016_1709r4
_cod_depositor_comments
'Adding full bibliography for 7045431--7045436.cif.'
_cod_database_code               7045436
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              24247