#------------------------------------------------------------------------------
#$Date: 2019-11-17 12:07:58 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229785 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/54/7045432.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7045432
loop_
_publ_author_name
'Chang, Yao-Pang'
'Hector, Andrew L.'
'Levason, William'
'Reid, Gillian'
'Whittam, Joshua'
_publ_section_title
;
 Synthesis and properties of MoCl₄ complexes with thio- and
 seleno-ethers and their use for chemical vapour deposition of
 MoSe₂ and MoS₂ 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 H12 Cl4 Mo S2'
_chemical_formula_sum            'C4 H12 Cl4 Mo S2'
_chemical_formula_weight         362.00
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7754(4)
_cell_length_b                   8.6531(4)
_cell_length_c                   13.0339(7)
_cell_measurement_reflns_used    3973
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.3330
_cell_measurement_theta_min      3.3800
_cell_volume                     1215.29(10)
_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 ω-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5273
_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         25.999
_diffrn_reflns_theta_min         3.126
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    2.248
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84168
_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            red
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2'
_exptl_crystal_size_max          0.039
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         1195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0208
_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/[σ²(Fo²)+(0.0236P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0439
_refine_ls_wR_factor_ref         0.0457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1032
_reflns_number_total             1195
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt04352j2.cif
_cod_data_source_block           2016_0210r2
_cod_depositor_comments
'Adding full bibliography for 7045431--7045436.cif.'
_cod_database_code               7045432
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.917
_shelx_estimated_absorpt_t_max   0.938
_shelx_res_file
; 
  
    2016_0210r2.res created by SHELXL-2014/7 
  
  
TITL 2016_0210r2 in Pbca 
CELL 0.71073  10.7754   8.6531  13.0339  90.000  90.000  90.000 
ZERR    4.00   0.0004   0.0004   0.0007   0.000   0.000   0.000 
LATT 1 
SYMM 0.5-X, -Y, 0.5+Z 
SYMM -X, 0.5+Y, 0.5-Z 
SYMM 0.5+X, 0.5-Y, -Z 
SFAC C  H  S  Cl Mo 
UNIT 16 48 8 16 4 
OMIT  -4.00  52.00 
L.S. 4 
ACTA 
BOND $H 
FMAP 2 
PLAN 5 
SIZE 0.029 0.031 0.039 
TEMP -173 
WGHT    0.023600 
FVAR       2.76946 
MOLE 1 
MO1   5    0.000000    0.000000    0.500000    10.50000    0.00988    0.01246 = 
         0.00780   -0.00069   -0.00120    0.00099 
S1    3    0.015953    0.167839    0.341632    11.00000    0.01342    0.02000 = 
         0.01115    0.00369   -0.00153   -0.00142 
CL1   4    0.203906    0.061550    0.547980    11.00000    0.01192    0.02304 = 
         0.01598    0.00071   -0.00280   -0.00184 
CL2   4   -0.071241    0.210220    0.595259    11.00000    0.01959    0.01831 = 
         0.01603   -0.00512    0.00005    0.00486 
C1    1    0.155704    0.114346    0.273531    11.00000    0.01824    0.02975 = 
         0.01522    0.00067    0.00312   -0.00206 
AFIX 137 
H1A   2    0.165775    0.181248    0.213438    11.00000   -1.50000 
H1B   2    0.149584    0.006449    0.251245    11.00000   -1.50000 
H1C   2    0.227490    0.126349    0.319003    11.00000   -1.50000 
AFIX   0 
C2    1    0.060199    0.359654    0.381506    11.00000    0.02647    0.01763 = 
         0.02563    0.00572   -0.00069   -0.00314 
AFIX 137 
H2A   2    0.133170    0.353493    0.426196    11.00000   -1.50000 
H2B   2   -0.008587    0.407586    0.419014    11.00000   -1.50000 
H2C   2    0.080056    0.422117    0.320974    11.00000   -1.50000 
AFIX   0 
HKLF 4 
  
REM  2016_0210r2 in Pbca 
REM R1 =  0.0208 for    1032 Fo > 4sig(Fo)  and  0.0270 for all    1195 data 
REM     54 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0236      0.0000 
  
REM Highest difference peak  0.447,  deepest hole -0.303,  1-sigma level  0.079 
Q1    1   0.0035  0.1134  0.4055  11.00000  0.05    0.45 
Q2    1  -0.0062 -0.0034  0.4313  11.00000  0.05    0.36 
Q3    1  -0.0538  0.1661  0.3097  11.00000  0.05    0.30 
Q4    1   0.0764  0.1394  0.3008  11.00000  0.05    0.29 
Q5    1  -0.0185  0.1696  0.6529  11.00000  0.05    0.27 
;
_shelx_res_checksum              95669
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Mo1 Mo 0.0000 0.0000 0.5000 0.01005(9) Uani 1 2 d S . P
S1 S 0.01595(5) 0.16784(7) 0.34163(4) 0.01485(14) Uani 1 1 d . . .
Cl1 Cl 0.20391(5) 0.06155(7) 0.54798(4) 0.01698(14) Uani 1 1 d . . .
Cl2 Cl -0.07124(5) 0.21022(6) 0.59526(4) 0.01798(14) Uani 1 1 d . . .
C1 C 0.1557(2) 0.1143(3) 0.27353(17) 0.0211(6) Uani 1 1 d . . .
H1A H 0.1658 0.1812 0.2134 0.032 Uiso 1 1 calc R U .
H1B H 0.1496 0.0064 0.2512 0.032 Uiso 1 1 calc R U .
H1C H 0.2275 0.1263 0.3190 0.032 Uiso 1 1 calc R U .
C2 C 0.0602(2) 0.3597(3) 0.38151(19) 0.0232(6) Uani 1 1 d . . .
H2A H 0.1332 0.3535 0.4262 0.035 Uiso 1 1 calc R U .
H2B H -0.0086 0.4076 0.4190 0.035 Uiso 1 1 calc R U .
H2C H 0.0801 0.4221 0.3210 0.035 Uiso 1 1 calc R U .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.00988(14) 0.01246(16) 0.00780(15) -0.00069(11) -0.00120(9) 0.00099(10)
S1 0.0134(3) 0.0200(3) 0.0111(3) 0.0037(2) -0.0015(2) -0.0014(2)
Cl1 0.0119(3) 0.0230(3) 0.0160(3) 0.0007(3) -0.0028(2) -0.0018(2)
Cl2 0.0196(3) 0.0183(3) 0.0160(3) -0.0051(2) 0.0000(2) 0.0049(2)
C1 0.0182(12) 0.0298(15) 0.0152(12) 0.0007(11) 0.0031(10) -0.0021(10)
C2 0.0265(13) 0.0176(13) 0.0256(14) 0.0057(11) -0.0007(11) -0.0031(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Cl2 Mo1 Cl2 180.0 . 5_556
Cl2 Mo1 Cl1 90.62(2) . 5_556
Cl2 Mo1 Cl1 89.39(2) 5_556 5_556
Cl2 Mo1 Cl1 89.39(2) . .
Cl2 Mo1 Cl1 90.61(2) 5_556 .
Cl1 Mo1 Cl1 180.0 5_556 .
Cl2 Mo1 S1 90.51(2) . .
Cl2 Mo1 S1 89.49(2) 5_556 .
Cl1 Mo1 S1 88.651(18) 5_556 .
Cl1 Mo1 S1 91.349(18) . .
Cl2 Mo1 S1 89.49(2) . 5_556
Cl2 Mo1 S1 90.51(2) 5_556 5_556
Cl1 Mo1 S1 91.349(18) 5_556 5_556
Cl1 Mo1 S1 88.651(18) . 5_556
S1 Mo1 S1 180.0 . 5_556
C2 S1 C1 99.03(11) . .
C2 S1 Mo1 108.13(8) . .
C1 S1 Mo1 108.07(8) . .
S1 C1 H1A 109.5 . .
S1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
S1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
S1 C2 H2A 109.5 . .
S1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
S1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 Cl2 2.3323(5) .
Mo1 Cl2 2.3324(5) 5_556
Mo1 Cl1 2.3457(5) 5_556
Mo1 Cl1 2.3457(5) .
Mo1 S1 2.5297(6) .
Mo1 S1 2.5298(6) 5_556
S1 C2 1.803(2) .
S1 C1 1.808(2) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
