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#$Date: 2019-11-17 12:07:58 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229785 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/54/7045431.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_7045431
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 H6 Cl4 Mo N2'
_chemical_formula_sum            'C4 H6 Cl4 Mo N2'
_chemical_formula_weight         319.85
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 102.276(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.622(9)
_cell_length_b                   7.507(4)
_cell_length_c                   5.825(4)
_cell_measurement_reflns_used    1021
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     496.6(6)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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  0.0637
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5422
_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         25.996
_diffrn_reflns_theta_min         3.253
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    2.336
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan. 
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.139
_exptl_crystal_description       Block
_exptl_crystal_F_000             308
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN'
_exptl_crystal_size_max          0.068
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0231
_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)+(0.0335P)²+0.0464P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                493
_reflns_number_total             534
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt04352j2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7045431--7045436.cif.'
_cod_database_code               7045431
_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   0.857
_shelx_estimated_absorpt_t_max   0.931
_shelx_res_file
; 
  
    shelx.res created by SHELXL-2014/7 
  
  
TITL shelx in C2/m 
CELL 0.71073 11.622 7.507 5.825 90 102.276 90 
ZERR 2 0.009 0.004 0.004 0 0.018 0 
LATT 7 
SYMM -X,+Y,-Z 
SFAC C  Cl Mo N  H 
UNIT 8 8 2 4 12 
OMIT  -4.00  52.00 
L.S. 5 
ACTA 
BOND $H 
TEMP -173 
SIZE 0.031 0.062 0.068 
FMAP 2 
PLAN 5 
CONF 
MORE -1 
TWIN 0 0 -1.994 0 -1 0 -0.502 0 -0.003 2 
WGHT    0.033500    0.046400 
BASF   0.44096 
FVAR       2.88759 
MO1   3    0.500000    0.000000    0.500000    10.25000    0.01773    0.02053 = 
         0.02322    0.00000    0.00350    0.00000 
CL1   2    0.408396    0.221120    0.679730    11.00000    0.02396    0.02539 = 
         0.02797   -0.00300    0.00551    0.00147 
N1    4    0.353810    0.000000    0.213535    10.50000    0.01857    0.02267 = 
         0.02670    0.00000    0.00162    0.00000 
C1    1    0.273235    0.000000    0.061319    10.50000    0.02507    0.01623 = 
         0.03174    0.00000    0.01110    0.00000 
C2    1    0.170359    0.000000   -0.132648    10.50000    0.02534    0.02530 = 
         0.02097    0.00000    0.00103    0.00000 
PART -1 
AFIX 137 
H2A   5    0.190778    0.056076   -0.270606    10.50000   -1.50000 
H2B   5    0.106369    0.066846   -0.086854    10.50000   -1.50000 
H2C   5    0.144875   -0.122922   -0.170680    10.50000   -1.50000 
PART 0 
AFIX   0 
HKLF 4 1 -1 1 1 1 0 0 0 0.5 -0.5 
  
REM  shelx in C2/m 
REM R1 =  0.0231 for     493 Fo > 4sig(Fo)  and  0.0256 for all     534 data 
REM     34 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0335      0.0592 
  
REM Highest difference peak  0.571,  deepest hole -0.293,  1-sigma level  0.094 
Q1    1   0.4595  0.1141  0.5860  11.00000  0.05    0.57 
Q2    1  -0.0121  0.0000 -0.3844  10.50000  0.05    0.57 
Q3    1   0.4518  0.0695  0.3867  11.00000  0.05    0.41 
Q4    1   0.4188  0.0000  0.5271  10.50000  0.05    0.37 
Q5    1   0.4352  0.3210  0.6089  11.00000  0.05    0.36 
;
_shelx_res_checksum              88151
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.5000 0.0000 0.5000 0.02062(17) Uani 1 4 d S T P . .
Cl1 Cl 0.40840(14) 0.22112(8) 0.6797(3) 0.0258(2) Uani 1 1 d . . . . .
N1 N 0.3538(4) 0.0000 0.2135(8) 0.0231(6) Uani 1 2 d S T P . .
C1 C 0.2732(4) 0.0000 0.0613(8) 0.0236(8) Uani 1 2 d S T P . .
C2 C 0.1704(5) 0.0000 -0.1326(10) 0.0244(9) Uani 1 2 d S T P . .
H2A H 0.1908 0.0561 -0.2706 0.037 Uiso 0.5 1 calc R U P A -1
H2B H 0.1064 0.0668 -0.0869 0.037 Uiso 0.5 1 calc R U P A -1
H2C H 0.1449 -0.1229 -0.1707 0.037 Uiso 0.5 1 calc R U P A -1
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 0.0177(3) 0.0205(2) 0.0232(3) 0.000 0.00350(17) 0.000
Cl1 0.0240(5) 0.0254(4) 0.0280(6) -0.0030(5) 0.0055(3) 0.0015(5)
N1 0.019(2) 0.0227(15) 0.027(3) 0.000 0.0016(13) 0.000
C1 0.025(2) 0.0162(14) 0.032(3) 0.000 0.0111(17) 0.000
C2 0.025(3) 0.0253(18) 0.021(3) 0.000 0.0010(16) 0.000
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'
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'
N N 0.0061 0.0033 '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'
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
N1 Mo1 N1 180.0 5_656 .
N1 Mo1 Cl1 90.72(13) 5_656 .
N1 Mo1 Cl1 89.28(13) . .
N1 Mo1 Cl1 90.72(13) 5_656 6
N1 Mo1 Cl1 89.28(13) . 6
Cl1 Mo1 Cl1 90.55(5) . 6
N1 Mo1 Cl1 89.28(13) 5_656 2_656
N1 Mo1 Cl1 90.72(13) . 2_656
Cl1 Mo1 Cl1 89.45(5) . 2_656
Cl1 Mo1 Cl1 180.0 6 2_656
N1 Mo1 Cl1 89.28(13) 5_656 5_656
N1 Mo1 Cl1 90.72(13) . 5_656
Cl1 Mo1 Cl1 180.0 . 5_656
Cl1 Mo1 Cl1 89.45(5) 6 5_656
Cl1 Mo1 Cl1 90.55(5) 2_656 5_656
C1 N1 Mo1 178.7(5) . .
N1 C1 C2 179.9(6) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 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 N1 2.113(3) 5_656
Mo1 N1 2.113(3) .
Mo1 Cl1 2.3364(10) .
Mo1 Cl1 2.3365(10) 6
Mo1 Cl1 2.3365(10) 2_656
Mo1 Cl1 2.3365(10) 5_656
N1 C1 1.145(4) .
C1 C2 1.460(5) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
