# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1557208'
_audit_update_record             
;
2017-06-20 deposited with the CCDC.
2017-12-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H6 Cl4 Mo N2'
_chemical_formula_sum            'C4 H6 Cl4 Mo N2'
_chemical_formula_weight         319.85

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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. 
;

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'

_cell_length_a                   11.622(9)
_cell_length_b                   7.507(4)
_cell_length_c                   5.825(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.276(18)
_cell_angle_gamma                90
_cell_volume                     496.6(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1021
_cell_measurement_theta_min      3.3
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.139
_exptl_crystal_F_000             308
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.068
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.031
_exptl_absorpt_coefficient_mu    2.336
_shelx_estimated_absorpt_T_min   0.857
_shelx_estimated_absorpt_T_max   0.931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
; 
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            5422
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.253
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             534
_reflns_number_gt                493
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refined as a 2-component twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0335P)²+0.0464P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         534
_refine_ls_number_parameters     34
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0231
_refine_ls_wR_factor_ref         0.0579
_refine_ls_wR_factor_gt          0.0570
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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 . ?

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
_geom_angle_publ_flag
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 . . ?


_refine_diff_density_max         0.571
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.094


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CH3CN'
_chemical_properties_physical    
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2016_0210r2
_database_code_depnum_ccdc_archive 'CCDC 1557209'
_audit_update_record             
;
2017-06-20 deposited with the CCDC.
2017-12-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H12 Cl4 Mo S2'
_chemical_formula_sum            'C4 H12 Cl4 Mo S2'
_chemical_formula_weight         362.00

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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. 
;

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'

_cell_length_a                   10.7754(4)
_cell_length_b                   8.6531(4)
_cell_length_c                   13.0339(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1215.29(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3973
_cell_measurement_theta_min      3.3800
_cell_measurement_theta_max      32.3330

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_F_000             712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.039
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.029
_exptl_absorpt_coefficient_mu    2.248
_shelx_estimated_absorpt_T_min   0.917
_shelx_estimated_absorpt_T_max   0.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84168
_exptl_absorpt_correction_T_max  1.00000
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            5273
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.126
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1195
_reflns_number_gt                1032
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0236P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1195
_refine_ls_number_parameters     54
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0208
_refine_ls_wR_factor_ref         0.0457
_refine_ls_wR_factor_gt          0.0439
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.0000 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 . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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 . ?

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
_geom_angle_publ_flag
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 . . ?

_refine_diff_density_max         0.447
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.079


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH2Cl2'
_chemical_properties_physical    
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2016_0110k1
_database_code_depnum_ccdc_archive 'CCDC 1557212'
_audit_update_record             
;
2017-06-20 deposited with the CCDC.
2017-12-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 H12 Cl4 Mo S2'
_chemical_formula_sum            'C5 H12 Cl4 Mo S2'
_chemical_formula_weight         374.01

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.9578(3)
_cell_length_b                   7.3230(2)
_cell_length_c                   12.5840(5)
_cell_angle_alpha                77.467(3)
_cell_angle_beta                 81.727(3)
_cell_angle_gamma                72.082(3)
_cell_volume                     593.49(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10851
_cell_measurement_theta_min      2.9550
_cell_measurement_theta_max      31.9830

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.093
_exptl_crystal_F_000             368
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.069
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.041
_exptl_absorpt_coefficient_mu    2.305
_shelx_estimated_absorpt_T_min   0.857
_shelx_estimated_absorpt_T_max   0.911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91261
_exptl_absorpt_correction_T_max  1.00000
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Left)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            12279
_diffrn_reflns_av_unetI/netI     0.0127
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.663
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2335
_reflns_number_gt                2161
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0264P)²+0.6851P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2335
_refine_ls_number_parameters     111
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0194
_refine_ls_wR_factor_ref         0.0528
_refine_ls_wR_factor_gt          0.0516
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.73800(3) 0.62606(3) 0.25019(2) 0.01511(7) Uani 1 1 d . . . . .
S1 S 0.82992(9) 0.41456(8) 0.10571(4) 0.01714(13) Uani 1 1 d . . . . .
S2 S 0.98650(9) 0.40315(8) 0.38522(5) 0.01624(12) Uani 1 1 d . . . . .
Cl1 Cl 0.52924(9) 0.84436(8) 0.12302(5) 0.02273(13) Uani 1 1 d . . . . .
Cl2 Cl 0.65384(9) 0.84475(8) 0.37263(5) 0.02081(13) Uani 1 1 d . . . . .
Cl3 Cl 0.52242(9) 0.45014(9) 0.33260(5) 0.02511(14) Uani 1 1 d . . . . .
Cl4 Cl 1.04275(9) 0.68738(8) 0.17154(5) 0.01985(13) Uani 1 1 d . . . . .
C1 C 0.6435(4) 0.2887(4) 0.1113(2) 0.0262(6) Uani 1 1 d . . . . .
H1A H 0.6755 0.2158 0.0512 0.039 Uiso 1 1 calc R U . . .
H1B H 0.5092 0.3836 0.1046 0.039 Uiso 1 1 calc R U . . .
H1C H 0.6438 0.1979 0.1812 0.039 Uiso 1 1 calc R U . . .
C2 C 1.0519(4) 0.2103(3) 0.13592(19) 0.0212(5) Uani 1 1 d . . . . .
H2A H 1.0542 0.1110 0.0931 0.025 Uiso 1 1 calc R U . . .
H2B H 1.1730 0.2562 0.1093 0.025 Uiso 1 1 calc R U . . .
C3 C 1.0727(4) 0.1102(3) 0.25460(19) 0.0198(5) Uani 1 1 d . . . . .
H3A H 0.9372 0.1039 0.2892 0.024 Uiso 1 1 calc R U . . .
H3B H 1.1601 -0.0256 0.2568 0.024 Uiso 1 1 calc R U . . .
C4 C 1.1607(3) 0.2095(3) 0.3212(2) 0.0191(5) Uani 1 1 d . . . . .
H4A H 1.2630 0.2640 0.2730 0.023 Uiso 1 1 calc R U . . .
H4B H 1.2332 0.1081 0.3793 0.023 Uiso 1 1 calc R U . . .
C5 C 0.8627(4) 0.2639(4) 0.49225(19) 0.0231(5) Uani 1 1 d . . . . .
H5A H 0.8091 0.1797 0.4611 0.035 Uiso 1 1 calc R U . . .
H5B H 0.7510 0.3526 0.5294 0.035 Uiso 1 1 calc R U . . .
H5C H 0.9601 0.1831 0.5449 0.035 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 Cl3 2.2686(6) . ?
Mo1 Cl1 2.3143(6) . ?
Mo1 Cl4 2.3380(6) . ?
Mo1 Cl2 2.3486(6) . ?
Mo1 S1 2.5282(6) . ?
Mo1 S2 2.5390(6) . ?
S1 C1 1.794(2) . ?
S1 C2 1.808(2) . ?
S2 C5 1.791(2) . ?
S2 C4 1.813(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.520(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.514(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?

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
_geom_angle_publ_flag
Cl3 Mo1 Cl1 98.40(2) . . ?
Cl3 Mo1 Cl4 158.22(2) . . ?
Cl1 Mo1 Cl4 97.61(2) . . ?
Cl3 Mo1 Cl2 96.29(2) . . ?
Cl1 Mo1 Cl2 92.82(2) . . ?
Cl4 Mo1 Cl2 97.58(2) . . ?
Cl3 Mo1 S1 87.41(2) . . ?
Cl1 Mo1 S1 83.61(2) . . ?
Cl4 Mo1 S1 79.79(2) . . ?
Cl2 Mo1 S1 175.21(2) . . ?
Cl3 Mo1 S2 86.13(2) . . ?
Cl1 Mo1 S2 175.42(2) . . ?
Cl4 Mo1 S2 78.20(2) . . ?
Cl2 Mo1 S2 85.94(2) . . ?
S1 Mo1 S2 97.370(19) . . ?
C1 S1 C2 100.53(12) . . ?
C1 S1 Mo1 110.55(9) . . ?
C2 S1 Mo1 111.52(8) . . ?
C5 S2 C4 100.43(11) . . ?
C5 S2 Mo1 110.94(9) . . ?
C4 S2 Mo1 109.51(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 . . ?
C3 C2 S1 117.46(17) . . ?
C3 C2 H2A 107.9 . . ?
S1 C2 H2A 107.9 . . ?
C3 C2 H2B 107.9 . . ?
S1 C2 H2B 107.9 . . ?
H2A C2 H2B 107.2 . . ?
C4 C3 C2 114.5(2) . . ?
C4 C3 H3A 108.6 . . ?
C2 C3 H3A 108.6 . . ?
C4 C3 H3B 108.6 . . ?
C2 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C3 C4 S2 117.57(16) . . ?
C3 C4 H4A 107.9 . . ?
S2 C4 H4A 107.9 . . ?
C3 C4 H4B 107.9 . . ?
S2 C4 H4B 107.9 . . ?
H4A C4 H4B 107.2 . . ?
S2 C5 H5A 109.5 . . ?
S2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
S2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

_refine_diff_density_max         0.511
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.081


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH2Cl2'
_chemical_properties_physical    
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2017_1201r1
_database_code_depnum_ccdc_archive 'CCDC 1557211'
_audit_update_record             
;
2017-06-20 deposited with the CCDC.
2017-12-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H18 Cl4 Mo S2'
_chemical_formula_sum            'C8 H18 Cl4 Mo S2'
_chemical_formula_weight         416.08

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.6773(2)
_cell_length_b                   9.1092(2)
_cell_length_c                   19.7049(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.465(2)
_cell_angle_gamma                90
_cell_volume                     1540.57(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11930
_cell_measurement_theta_min      2.1730
_cell_measurement_theta_max      32.3180

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_F_000             832
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.107
_exptl_absorpt_coefficient_mu    1.786
_shelx_estimated_absorpt_T_min   0.755
_shelx_estimated_absorpt_T_max   0.832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87713
_exptl_absorpt_correction_T_max  1.00000
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            12891
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.468
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3018
_reflns_number_gt                2979
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0093P)²+4.0664P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3018
_refine_ls_number_parameters     140
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0577
_refine_ls_wR_factor_gt          0.0575
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_restrained_S_all      1.224
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.20270(3) 0.22597(3) 0.14737(2) 0.01344(7) Uani 1 1 d . . . . .
Cl1 Cl 0.45728(8) 0.20102(8) 0.12597(4) 0.01994(15) Uani 1 1 d . . . . .
Cl2 Cl 0.23442(9) 0.45876(7) 0.19638(4) 0.02293(16) Uani 1 1 d . . . . .
Cl3 Cl -0.03196(7) 0.17305(7) 0.18450(3) 0.01703(14) Uani 1 1 d . . . . .
Cl4 Cl 0.10158(9) 0.31612(8) 0.04098(4) 0.02520(16) Uani 1 1 d . . . . .
S1 S 0.33709(8) 0.11256(7) 0.26126(3) 0.01451(14) Uani 1 1 d . . . . .
S2 S 0.16300(7) -0.04252(7) 0.10811(3) 0.01328(14) Uani 1 1 d . . . . .
C1 C 0.2011(4) 0.2582(3) 0.35460(15) 0.0233(6) Uani 1 1 d . . . . .
H1A H 0.1281 0.2619 0.3881 0.035 Uiso 1 1 calc R U . . .
H1B H 0.1653 0.3246 0.3164 0.035 Uiso 1 1 calc R U . . .
H1C H 0.3048 0.2885 0.3767 0.035 Uiso 1 1 calc R U . . .
C2 C 0.2087(3) 0.1020(3) 0.32761(13) 0.0175(6) Uani 1 1 d . . . . .
H2 H 0.1024 0.0695 0.3064 0.021 Uiso 1 1 calc R U . . .
C3 C 0.2729(3) -0.0036(3) 0.38426(14) 0.0208(6) Uani 1 1 d . . . . .
H3A H 0.3804 0.0237 0.4023 0.031 Uiso 1 1 calc R U . . .
H3B H 0.2710 -0.1036 0.3659 0.031 Uiso 1 1 calc R U . . .
H3C H 0.2088 0.0009 0.4212 0.031 Uiso 1 1 calc R U . . .
C4 C 0.3548(3) -0.0760(3) 0.23375(14) 0.0185(6) Uani 1 1 d . . . . .
H4A H 0.4427 -0.0828 0.2070 0.022 Uiso 1 1 calc R U . . .
H4B H 0.3798 -0.1391 0.2748 0.022 Uiso 1 1 calc R U . . .
C5 C 0.2095(4) -0.1334(3) 0.19060(14) 0.0186(6) Uani 1 1 d . . . . .
H5A H 0.1207 -0.1215 0.2164 0.022 Uiso 1 1 calc R U . . .
H5B H 0.2226 -0.2398 0.1828 0.022 Uiso 1 1 calc R U . . .
C6 C 0.3126(4) -0.2743(3) 0.05390(16) 0.0240(6) Uani 1 1 d . . . . .
H6A H 0.2067 -0.3077 0.0366 0.036 Uiso 1 1 calc R U . . .
H6B H 0.3466 -0.3174 0.0992 0.036 Uiso 1 1 calc R U . . .
H6C H 0.3835 -0.3049 0.0222 0.036 Uiso 1 1 calc R U . . .
C7 C 0.3141(3) -0.1082(3) 0.05971(13) 0.0150(5) Uani 1 1 d . . . . .
H7 H 0.4184 -0.0755 0.0833 0.018 Uiso 1 1 calc R U . . .
C8 C 0.2802(4) -0.0342(4) -0.01030(14) 0.0225(6) Uani 1 1 d . . . . .
H8A H 0.3583 -0.0647 -0.0387 0.034 Uiso 1 1 calc R U . . .
H8B H 0.2842 0.0726 -0.0044 0.034 Uiso 1 1 calc R U . . .
H8C H 0.1763 -0.0630 -0.0328 0.034 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 Cl4 2.3016(7) . ?
Mo1 Cl3 2.3135(7) . ?
Mo1 Cl1 2.3203(7) . ?
Mo1 Cl2 2.3295(7) . ?
Mo1 S2 2.5730(7) . ?
Mo1 S1 2.5872(7) . ?
S1 C4 1.814(3) . ?
S1 C2 1.841(3) . ?
S2 C5 1.816(3) . ?
S2 C7 1.832(3) . ?
C1 C2 1.524(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.516(4) . ?
C2 H2 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.507(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.517(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.525(4) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?

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
_geom_angle_publ_flag
Cl4 Mo1 Cl3 97.30(3) . . ?
Cl4 Mo1 Cl1 96.60(3) . . ?
Cl3 Mo1 Cl1 160.54(3) . . ?
Cl4 Mo1 Cl2 93.37(3) . . ?
Cl3 Mo1 Cl2 96.57(3) . . ?
Cl1 Mo1 Cl2 96.14(3) . . ?
Cl4 Mo1 S2 92.81(3) . . ?
Cl3 Mo1 S2 79.16(2) . . ?
Cl1 Mo1 S2 86.63(2) . . ?
Cl2 Mo1 S2 172.89(2) . . ?
Cl4 Mo1 S1 174.44(3) . . ?
Cl3 Mo1 S1 87.01(2) . . ?
Cl1 Mo1 S1 78.40(2) . . ?
Cl2 Mo1 S1 89.61(2) . . ?
S2 Mo1 S1 84.52(2) . . ?
C4 S1 C2 104.44(13) . . ?
C4 S1 Mo1 99.55(9) . . ?
C2 S1 Mo1 113.23(9) . . ?
C5 S2 C7 103.60(13) . . ?
C5 S2 Mo1 99.33(9) . . ?
C7 S2 Mo1 113.12(9) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 111.4(2) . . ?
C3 C2 S1 111.17(19) . . ?
C1 C2 S1 105.14(19) . . ?
C3 C2 H2 109.7 . . ?
C1 C2 H2 109.7 . . ?
S1 C2 H2 109.7 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C4 S1 113.38(19) . . ?
C5 C4 H4A 108.9 . . ?
S1 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
S1 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
C4 C5 S2 113.83(19) . . ?
C4 C5 H5A 108.8 . . ?
S2 C5 H5A 108.8 . . ?
C4 C5 H5B 108.8 . . ?
S2 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C6 C7 C8 112.0(2) . . ?
C6 C7 S2 111.5(2) . . ?
C8 C7 S2 105.60(18) . . ?
C6 C7 H7 109.2 . . ?
C8 C7 H7 109.2 . . ?
S2 C7 H7 109.2 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

_refine_diff_density_max         0.680
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.085


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH2Cl2'
_chemical_properties_physical    
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2016_1709r2
_database_code_depnum_ccdc_archive 'CCDC 1557213'
_audit_update_record             
;
2017-06-20 deposited with the CCDC.
2017-12-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H17 Cl5 Mo S3'
_chemical_formula_sum            'C6 H17 Cl5 Mo S3'
_chemical_formula_weight         458.57

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   11.1611(3)
_cell_length_b                   23.6764(11)
_cell_length_c                   12.6813(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3351.1(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9256
_cell_measurement_theta_min      2.5000
_cell_measurement_theta_max      32.1950

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_F_000             1824
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.034
_exptl_absorpt_coefficient_mu    1.925
_shelx_estimated_absorpt_T_min   0.778
_shelx_estimated_absorpt_T_max   0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87762
_exptl_absorpt_correction_T_max  1.00000
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            14898
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.822
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             6472
_reflns_number_gt                5663
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.879
_reflns_Friedel_fraction_max     0.967
_reflns_Friedel_fraction_full    0.973

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0332P)²+2.0347P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 2286 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.12(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6472
_refine_ls_number_parameters     281
_refine_ls_number_restraints     184
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0735
_refine_ls_wR_factor_gt          0.0700
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.45137(4) 0.37125(2) 0.12266(5) 0.01289(13) Uani 1 1 d . U . . .
Cl1 Cl 0.39341(15) 0.32305(7) -0.03117(13) 0.0185(4) Uani 1 1 d . U . . .
Cl2 Cl 0.61803(14) 0.40796(7) 0.02642(13) 0.0173(4) Uani 1 1 d . U . . .
Cl3 Cl 0.50846(16) 0.42818(8) 0.26727(13) 0.0239(4) Uani 1 1 d . U . . .
Cl4 Cl 0.28226(15) 0.33950(8) 0.21182(13) 0.0211(4) Uani 1 1 d . U . . .
Cl5 Cl 0.56489(14) 0.29248(8) 0.18391(14) 0.0187(4) Uani 1 1 d . U . . .
S1 S 0.34364(16) 0.46098(8) 0.06347(14) 0.0188(4) Uani 1 1 d . U . . .
C1 C 0.3178(8) 0.4609(4) -0.0749(6) 0.035(2) Uani 1 1 d . U . . .
H1A H 0.2675 0.4285 -0.0937 0.053 Uiso 1 1 calc R U . . .
H1B H 0.3946 0.4583 -0.1121 0.053 Uiso 1 1 calc R U . . .
H1C H 0.2771 0.4960 -0.0952 0.053 Uiso 1 1 calc R U . . .
C2 C 0.1927(6) 0.4583(3) 0.1101(7) 0.0372(17) Uani 1 1 d . U . . .
H2A H 0.1528 0.4943 0.0952 0.056 Uiso 1 1 calc R U . . .
H2B H 0.1926 0.4514 0.1863 0.056 Uiso 1 1 calc R U . . .
H2C H 0.1498 0.4276 0.0744 0.056 Uiso 1 1 calc R U . . .
Mo2 Mo 0.08806(4) 0.37611(2) 0.62266(5) 0.01222(13) Uani 1 1 d . U . . .
Cl6 Cl 0.02269(16) 0.43438(8) 0.76240(13) 0.0209(4) Uani 1 1 d . U . . .
Cl7 Cl -0.08368(14) 0.40723(7) 0.52546(13) 0.0173(4) Uani 1 1 d . U . . .
Cl8 Cl 0.14968(15) 0.32825(7) 0.46995(12) 0.0171(4) Uani 1 1 d . U . . .
Cl9 Cl 0.25956(14) 0.34911(8) 0.71396(13) 0.0202(4) Uani 1 1 d . U . . .
Cl10 Cl -0.01813(14) 0.29619(7) 0.68873(13) 0.0173(4) Uani 1 1 d . U . . .
S2 S 0.20114(16) 0.46326(8) 0.55914(14) 0.0181(4) Uani 1 1 d . U . . .
C3 C 0.3536(7) 0.4438(4) 0.5365(8) 0.0389(18) Uani 1 1 d . U . . .
H3A H 0.3564 0.4094 0.4936 0.058 Uiso 1 1 calc R U . . .
H3B H 0.3934 0.4369 0.6042 0.058 Uiso 1 1 calc R U . . .
H3C H 0.3948 0.4744 0.4993 0.058 Uiso 1 1 calc R U . . .
C4 C 0.1587(8) 0.4773(4) 0.4260(7) 0.0442(19) Uani 1 1 d . U . . .
H4A H 0.2016 0.5108 0.4006 0.066 Uiso 1 1 calc R U . . .
H4B H 0.0722 0.4842 0.4227 0.066 Uiso 1 1 calc R U . . .
H4C H 0.1791 0.4448 0.3818 0.066 Uiso 1 1 calc R U . . .
S11 S 0.92483(16) 0.36086(8) -0.00629(14) 0.0182(4) Uani 1 1 d . U . . .
S12 S 0.93215(16) 0.34314(8) 0.22561(14) 0.0162(4) Uani 1 1 d . U . . .
C11 C 1.0630(6) 0.3225(3) -0.0288(6) 0.0216(16) Uani 1 1 d . U . . .
H11A H 1.1147 0.3259 0.0334 0.032 Uiso 1 1 calc R U . . .
H11B H 1.1042 0.3384 -0.0903 0.032 Uiso 1 1 calc R U . . .
H11C H 1.0449 0.2826 -0.0416 0.032 Uiso 1 1 calc R U . . .
C12 C 0.8666(6) 0.3204(3) 0.1005(5) 0.0152(15) Uani 1 1 d . U . . .
H12A H 0.8844 0.2800 0.0889 0.018 Uiso 1 1 calc R U . . .
H12B H 0.7784 0.3250 0.1034 0.018 Uiso 1 1 calc R U . . .
C13 C 0.8595(7) 0.4096(3) 0.2428(6) 0.0267(18) Uani 1 1 d . U . . .
H13A H 0.7725 0.4043 0.2398 0.040 Uiso 1 1 calc R U . . .
H13B H 0.8844 0.4354 0.1866 0.040 Uiso 1 1 calc R U . . .
H13C H 0.8816 0.4255 0.3114 0.040 Uiso 1 1 calc R U . . .
C14 C 0.8551(6) 0.2997(3) 0.3195(5) 0.0167(15) Uani 1 1 d . U . . .
H14A H 0.8754 0.3120 0.3910 0.025 Uiso 1 1 calc R U . . .
H14B H 0.8792 0.2603 0.3100 0.025 Uiso 1 1 calc R U . . .
H14C H 0.7684 0.3032 0.3087 0.025 Uiso 1 1 calc R U . . .
S13 S 0.61733(16) 0.35268(8) 0.49555(13) 0.0169(4) Uani 1 1 d . U . . .
S14 S 0.60689(15) 0.33470(8) 0.72720(13) 0.0156(4) Uani 1 1 d . U . . .
C15 C 0.4835(6) 0.3117(3) 0.4732(6) 0.0210(16) Uani 1 1 d . U . . .
H15A H 0.5049 0.2718 0.4653 0.032 Uiso 1 1 calc R U . . .
H15B H 0.4439 0.3250 0.4088 0.032 Uiso 1 1 calc R U . . .
H15C H 0.4291 0.3161 0.5333 0.032 Uiso 1 1 calc R U . . .
C16 C 0.6785(5) 0.3142(3) 0.6042(5) 0.0148(15) Uani 1 1 d . U . . .
H16A H 0.7657 0.3215 0.6089 0.018 Uiso 1 1 calc R U . . .
H16B H 0.6668 0.2732 0.5924 0.018 Uiso 1 1 calc R U . . .
C17 C 0.6682(7) 0.4043(3) 0.7433(6) 0.0269(18) Uani 1 1 d . U . . .
H17A H 0.6385 0.4207 0.8092 0.040 Uiso 1 1 calc R U . . .
H17B H 0.6438 0.4280 0.6838 0.040 Uiso 1 1 calc R U . . .
H17C H 0.7558 0.4020 0.7457 0.040 Uiso 1 1 calc R U . . .
C18 C 0.6906(6) 0.2951(3) 0.8227(6) 0.0200(16) Uani 1 1 d . U . . .
H18A H 0.7755 0.3054 0.8183 0.030 Uiso 1 1 calc R U . . .
H18B H 0.6816 0.2546 0.8085 0.030 Uiso 1 1 calc R U . . .
H18C H 0.6605 0.3035 0.8936 0.030 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 Cl4 2.3251(17) . ?
Mo1 Cl1 2.3509(17) . ?
Mo1 Cl3 2.3633(18) . ?
Mo1 Cl5 2.3847(18) . ?
Mo1 Cl2 2.3885(17) . ?
Mo1 S1 2.5538(19) . ?
S1 C1 1.778(8) . ?
S1 C2 1.787(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
Mo2 Cl9 2.3266(17) . ?
Mo2 Cl8 2.3468(17) . ?
Mo2 Cl6 2.3613(18) . ?
Mo2 Cl10 2.3847(18) . ?
Mo2 Cl7 2.3951(17) . ?
Mo2 S2 2.5496(19) . ?
S2 C4 1.784(8) . ?
S2 C3 1.787(8) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
S11 C12 1.781(6) . ?
S11 C11 1.812(7) . ?
S12 C13 1.783(7) . ?
S12 C14 1.792(7) . ?
S12 C12 1.828(6) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
S13 C16 1.787(6) . ?
S13 C15 1.803(7) . ?
S14 C18 1.795(7) . ?
S14 C17 1.795(8) . ?
S14 C16 1.819(6) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?

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
_geom_angle_publ_flag
Cl4 Mo1 Cl1 91.33(6) . . ?
Cl4 Mo1 Cl3 91.48(7) . . ?
Cl1 Mo1 Cl3 174.23(7) . . ?
Cl4 Mo1 Cl5 91.15(6) . . ?
Cl1 Mo1 Cl5 92.11(7) . . ?
Cl3 Mo1 Cl5 92.87(7) . . ?
Cl4 Mo1 Cl2 176.69(7) . . ?
Cl1 Mo1 Cl2 88.10(6) . . ?
Cl3 Mo1 Cl2 88.80(6) . . ?
Cl5 Mo1 Cl2 92.13(6) . . ?
Cl4 Mo1 S1 91.70(6) . . ?
Cl1 Mo1 S1 91.74(6) . . ?
Cl3 Mo1 S1 83.14(6) . . ?
Cl5 Mo1 S1 175.16(6) . . ?
Cl2 Mo1 S1 85.05(6) . . ?
C1 S1 C2 100.0(4) . . ?
C1 S1 Mo1 111.5(3) . . ?
C2 S1 Mo1 108.5(3) . . ?
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 . . ?
Cl9 Mo2 Cl8 92.11(6) . . ?
Cl9 Mo2 Cl6 92.36(6) . . ?
Cl8 Mo2 Cl6 172.72(7) . . ?
Cl9 Mo2 Cl10 90.92(6) . . ?
Cl8 Mo2 Cl10 93.01(6) . . ?
Cl6 Mo2 Cl10 92.66(7) . . ?
Cl9 Mo2 Cl7 177.52(7) . . ?
Cl8 Mo2 Cl7 87.62(6) . . ?
Cl6 Mo2 Cl7 87.66(6) . . ?
Cl10 Mo2 Cl7 91.56(6) . . ?
Cl9 Mo2 S2 88.41(6) . . ?
Cl8 Mo2 S2 89.14(6) . . ?
Cl6 Mo2 S2 85.25(6) . . ?
Cl10 Mo2 S2 177.77(7) . . ?
Cl7 Mo2 S2 89.12(6) . . ?
C4 S2 C3 98.6(5) . . ?
C4 S2 Mo2 108.6(3) . . ?
C3 S2 Mo2 108.3(3) . . ?
S2 C3 H3A 109.5 . . ?
S2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
S2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
S2 C4 H4A 109.5 . . ?
S2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
S2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C12 S11 C11 99.3(3) . . ?
C13 S12 C14 101.9(4) . . ?
C13 S12 C12 100.5(3) . . ?
C14 S12 C12 102.5(3) . . ?
S11 C11 H11A 109.5 . . ?
S11 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
S11 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
S11 C12 S12 110.8(3) . . ?
S11 C12 H12A 109.5 . . ?
S12 C12 H12A 109.5 . . ?
S11 C12 H12B 109.5 . . ?
S12 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
S12 C13 H13A 109.5 . . ?
S12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
S12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
S12 C14 H14A 109.5 . . ?
S12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
S12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 S13 C15 99.4(3) . . ?
C18 S14 C17 101.8(4) . . ?
C18 S14 C16 102.2(3) . . ?
C17 S14 C16 100.1(3) . . ?
S13 C15 H15A 109.5 . . ?
S13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
S13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
S13 C16 S14 110.9(3) . . ?
S13 C16 H16A 109.5 . . ?
S14 C16 H16A 109.5 . . ?
S13 C16 H16B 109.5 . . ?
S14 C16 H16B 109.5 . . ?
H16A C16 H16B 108.0 . . ?
S14 C17 H17A 109.5 . . ?
S14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
S14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
S14 C18 H18A 109.5 . . ?
S14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
S14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

_refine_diff_density_max         0.690
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.095


_chemical_properties_physical    
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2016_1709r4
_database_code_depnum_ccdc_archive 'CCDC 1557210'
_audit_update_record             
;
2017-06-20 deposited with the CCDC.
2017-12-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H10 Cl4 Mo S2'
_chemical_formula_sum            'C4 H10 Cl4 Mo S2'
_chemical_formula_weight         359.98

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   7.1386(6)
_cell_length_b                   11.1622(6)
_cell_length_c                   7.8033(7)
_cell_angle_alpha                90
_cell_angle_beta                 115.913(11)
_cell_angle_gamma                90
_cell_volume                     559.27(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3685
_cell_measurement_theta_min      2.8700
_cell_measurement_theta_max      32.3640

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.138
_exptl_crystal_F_000             352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.041
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.031
_exptl_absorpt_coefficient_mu    2.442
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.42069
_exptl_absorpt_correction_T_max  1.00000
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            5766
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.902
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2142
_reflns_number_gt                1903
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refined as a 2-component inversion twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0858P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   -0.13(16)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2142
_refine_ls_number_parameters     103
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1223
_refine_ls_wR_factor_gt          0.1177
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.69334(14) 0.07342(8) 0.25066(13) 0.0224(3) Uani 1 1 d . . . . .
Cl1 Cl 0.4253(4) 0.1730(2) 0.0082(4) 0.0251(6) Uani 1 1 d . . . . .
Cl2 Cl 0.9861(4) -0.0410(3) 0.4172(5) 0.0328(7) Uani 1 1 d . . . . .
Cl3 Cl 0.7037(5) 0.1859(3) 0.4934(5) 0.0329(7) Uani 1 1 d . . . . .
Cl4 Cl 0.4694(4) -0.0743(2) 0.2672(4) 0.0247(6) Uani 1 1 d . . . . .
S1 S 0.9086(4) 0.2327(2) 0.1921(4) 0.0223(6) Uani 1 1 d . . . . .
S2 S 0.7390(4) -0.0385(2) -0.0195(4) 0.0222(6) Uani 1 1 d . . . . .
C1 C 1.1798(18) 0.2125(10) 0.3508(19) 0.030(3) Uani 1 1 d . . . . .
H1A H 1.2173 0.1280 0.3512 0.045 Uiso 1 1 calc R U . . .
H1B H 1.2052 0.2366 0.4799 0.045 Uiso 1 1 calc R U . . .
H1C H 1.2645 0.2619 0.3077 0.045 Uiso 1 1 calc R U . . .
C2 C 0.8968(18) 0.1854(10) -0.0351(17) 0.024(2) Uani 1 1 d . . . . .
H2A H 0.7582 0.2065 -0.1373 0.029 Uiso 1 1 calc R U . . .
H2B H 1.0024 0.2306 -0.0589 0.029 Uiso 1 1 calc R U . . .
C3 C 0.9329(17) 0.0540(10) -0.0469(17) 0.028(3) Uani 1 1 d . . . . .
H3A H 1.0723 0.0328 0.0536 0.034 Uiso 1 1 calc R U . . .
H3B H 0.9318 0.0366 -0.1717 0.034 Uiso 1 1 calc R U . . .
C4 C 0.5140(17) -0.0192(10) -0.2443(17) 0.027(3) Uani 1 1 d . . . . .
H4A H 0.4917 0.0663 -0.2747 0.041 Uiso 1 1 calc R U . . .
H4B H 0.3913 -0.0529 -0.2362 0.041 Uiso 1 1 calc R U . . .
H4C H 0.5366 -0.0607 -0.3444 0.041 Uiso 1 1 calc R U . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 Cl3 2.247(3) . ?
Mo1 Cl1 2.305(3) . ?
Mo1 Cl2 2.305(3) . ?
Mo1 Cl4 2.339(3) . ?
Mo1 S1 2.519(3) . ?
Mo1 S2 2.591(3) . ?
S1 C1 1.799(12) . ?
S1 C2 1.816(12) . ?
S2 C4 1.800(11) . ?
S2 C3 1.813(12) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.499(15) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?

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
_geom_angle_publ_flag
Cl3 Mo1 Cl1 97.61(12) . . ?
Cl3 Mo1 Cl2 98.42(13) . . ?
Cl1 Mo1 Cl2 162.33(12) . . ?
Cl3 Mo1 Cl4 96.83(11) . . ?
Cl1 Mo1 Cl4 92.47(10) . . ?
Cl2 Mo1 Cl4 92.95(10) . . ?
Cl3 Mo1 S1 87.75(11) . . ?
Cl1 Mo1 S1 82.18(10) . . ?
Cl2 Mo1 S1 91.07(10) . . ?
Cl4 Mo1 S1 173.41(10) . . ?
Cl3 Mo1 S2 170.43(11) . . ?
Cl1 Mo1 S2 85.34(10) . . ?
Cl2 Mo1 S2 77.66(11) . . ?
Cl4 Mo1 S2 92.13(10) . . ?
S1 Mo1 S2 83.62(9) . . ?
C1 S1 C2 102.3(6) . . ?
C1 S1 Mo1 110.2(4) . . ?
C2 S1 Mo1 101.5(4) . . ?
C4 S2 C3 102.7(5) . . ?
C4 S2 Mo1 111.1(4) . . ?
C3 S2 Mo1 101.3(4) . . ?
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 . . ?
C3 C2 S1 114.1(8) . . ?
C3 C2 H2A 108.7 . . ?
S1 C2 H2A 108.7 . . ?
C3 C2 H2B 108.7 . . ?
S1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C2 C3 S2 112.9(8) . . ?
C2 C3 H3A 109.0 . . ?
S2 C3 H3A 109.0 . . ?
C2 C3 H3B 109.0 . . ?
S2 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
S2 C4 H4A 109.5 . . ?
S2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
S2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

_refine_diff_density_max         1.171
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.163


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH2Cl2'
_chemical_properties_physical    
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
