# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_moocl3(seme)2-1
_database_code_depnum_ccdc_archive 'CCDC 2050667'
loop_
_audit_author_name
_audit_author_address
'Danielle Smith'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2020-12-16 deposited with the CCDC.	2021-02-26 downloaded from the CCDC.
;
_audit_creation_date             2020-05-04
_audit_creation_method           
;
Olex2 1.3
(compiled Sep 10 2019 10:52:38 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[MoOCl2(SeMe2)2(Cl)2]'
_chemical_formula_moiety         'C4 H12 Cl6 Mo2 O2 Se2'
_chemical_formula_sum            'C4 H12 Cl6 Mo2 O2 Se2'
_chemical_formula_weight         654.64
_chemical_melting_point          ?
_chemical_oxdiff_formula         MoOCl3SeCH
_chemical_oxdiff_usercomment     'Yellow Plate'
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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   7.8374(2)
_cell_length_b                   9.6744(2)
_cell_length_c                   11.2666(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.647(3)
_cell_angle_gamma                90
_cell_volume                     822.60(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7885
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.1600
_cell_measurement_theta_min      2.6810
_shelx_estimated_absorpt_T_max   0.231
_shelx_estimated_absorpt_T_min   0.231
_exptl_absorpt_coefficient_mu    6.907
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.643
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             612
_exptl_crystal_preparation       'Slow evporation from Toluene'
_exptl_crystal_recrystallization_method 'Slow evporation from Toluene`'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.869
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11835
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.664
_diffrn_reflns_theta_min         2.699
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.8691
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -43.00 -16.00   0.50    0.50    --    5.00 -38.00 -30.00   54
  2  ω    -94.00   1.00   0.50    0.50    --   -8.40 -60.00 150.00  190
  3  ω    -35.00  19.00   0.50    0.50    --   -8.40 -60.00   0.00  108
  4  ω    -69.00  21.00   0.50    0.50    --   -8.40 -57.00-120.00  180
  5  ω    -97.00  40.00   0.50    0.50    --   -8.40 -19.00 -30.00  274
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0865456000
_diffrn_orient_matrix_UB_12      -0.0206024000
_diffrn_orient_matrix_UB_13      0.0008933000
_diffrn_orient_matrix_UB_21      -0.0367748000
_diffrn_orient_matrix_UB_22      0.0474389000
_diffrn_orient_matrix_UB_23      -0.0481164000
_diffrn_orient_matrix_UB_31      0.0007532000
_diffrn_orient_matrix_UB_32      -0.0519446000
_diffrn_orient_matrix_UB_33      -0.0442256000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2452
_reflns_number_total             2616
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         2616
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0167
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0120P)²+0.6276P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0348
_refine_ls_wR_factor_ref         0.0354
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C1(H1a,H1b,H1c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.65913(2) 0.65774(2) 0.58098(2) 0.00929(4) Uani 1 1 d . . . . .
Se1 Se 0.84390(2) 0.44671(2) 0.70387(2) 0.01070(4) Uani 1 1 d . . . . .
Cl1 Cl 0.39693(5) 0.54388(4) 0.60293(3) 0.01104(7) Uani 1 1 d . . . . .
Cl2 Cl 0.48086(5) 0.79832(4) 0.42816(4) 0.01482(8) Uani 1 1 d . . . . .
Cl3 Cl 0.90706(5) 0.69535(4) 0.50859(4) 0.01523(8) Uani 1 1 d . . . . .
O1 O 0.70027(15) 0.75685(13) 0.70500(11) 0.0153(2) Uani 1 1 d . . . . .
C2 C 1.0556(2) 0.54380(18) 0.79784(16) 0.0162(3) Uani 1 1 d . . . . .
H2A H 1.021583 0.627519 0.831138 0.024 Uiso 1 1 calc GR . . . .
H2B H 1.129045 0.565762 0.744683 0.024 Uiso 1 1 calc GR . . . .
H2C H 1.120183 0.485869 0.863931 0.024 Uiso 1 1 calc GR . . . .
C1 C 0.7326(2) 0.42441(19) 0.83813(16) 0.0171(3) Uani 1 1 d . . . . .
H1A H 0.804256 0.364995 0.900069 0.026 Uiso 1 1 calc GR . . . .
H1B H 0.617189 0.384192 0.806771 0.026 Uiso 1 1 calc GR . . . .
H1C H 0.721494 0.513073 0.873586 0.026 Uiso 1 1 calc GR . . . .

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 0.00934(6) 0.00855(7) 0.01001(6) -0.00020(4) 0.00266(5) -0.00123(4)
Se1 0.01042(7) 0.00992(8) 0.01168(8) -0.00070(5) 0.00284(6) 0.00058(5)
Cl1 0.01027(15) 0.01207(17) 0.01175(16) -0.00144(12) 0.00464(13) -0.00137(12)
Cl2 0.01549(17) 0.01219(17) 0.01591(18) 0.00392(14) 0.00276(14) 0.00090(13)
Cl3 0.01220(16) 0.01811(19) 0.01648(18) 0.00038(14) 0.00578(14) -0.00423(14)
O1 0.0177(5) 0.0140(6) 0.0143(5) -0.0029(4) 0.0043(5) -0.0023(4)
C2 0.0118(7) 0.0182(8) 0.0166(8) -0.0021(6) 0.0005(6) -0.0009(6)
C1 0.0164(7) 0.0209(8) 0.0153(8) 0.0053(6) 0.0064(6) 0.0033(6)

_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 Se1 2.6647(2) . ?
Mo1 Cl1 2.7927(4) 3_666 ?
Mo1 Cl1 2.4024(4) . ?
Mo1 Cl2 2.3385(4) . ?
Mo1 Cl3 2.3299(4) . ?
Mo1 O1 1.6532(12) . ?
Se1 C2 1.9513(16) . ?
Se1 C1 1.9514(17) . ?

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
Se1 Mo1 Cl1 78.763(9) . 3_666 ?
Cl1 Mo1 Se1 87.438(10) . . ?
Cl1 Mo1 Cl1 77.783(13) . 3_666 ?
Cl2 Mo1 Se1 163.988(12) . . ?
Cl2 Mo1 Cl1 85.225(13) . 3_666 ?
Cl2 Mo1 Cl1 89.123(14) . . ?
Cl3 Mo1 Se1 85.058(12) . . ?
Cl3 Mo1 Cl1 157.663(15) . . ?
Cl3 Mo1 Cl1 80.126(13) . 3_666 ?
Cl3 Mo1 Cl2 92.323(15) . . ?
O1 Mo1 Se1 92.89(4) . . ?
O1 Mo1 Cl1 171.11(4) . 3_666 ?
O1 Mo1 Cl1 98.98(4) . . ?
O1 Mo1 Cl2 103.09(4) . . ?
O1 Mo1 Cl3 102.38(4) . . ?
C2 Se1 Mo1 100.17(5) . . ?
C2 Se1 C1 97.19(8) . . ?
C1 Se1 Mo1 101.16(5) . . ?
Mo1 Cl1 Mo1 102.218(13) . 3_666 ?

_iucr_refine_instructions_details 
;
TITL moocl3(seme)2-1_a.res in P2(1)/c
    moocl3(seme)2-1.res
    created by SHELXL-2018/3 at 12:12:58 on 10-Feb-2020
REM Old TITL MoOCl3(SeMe)2-1 in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.030, Rweak 0.009, Alpha 0.013
REM <I/s> 0.782 for 109 systematic absences, Orientation as input
REM Formula found by SHELXT: C2 O Cl3 Se Mo
CELL 0.71073 7.8374 9.6744 11.2666 90 105.647 90
ZERR 2 0.0002 0.0002 0.0003 0 0.003 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl Mo O Se
UNIT 8 24 12 4 4 4

L.S. 4
PLAN  20
SIZE 0.3 0.3 0.3
BOND
list 4
fmap 2
ACTA
REM <olex2.extras>
REM <HklSrc "%.\\MoOCl3(SeMe)2-1.hkl">
REM </olex2.extras>

WGHT    0.012000    0.627600
FVAR       0.38220
MO1   4    0.659127    0.657736    0.580976    11.00000    0.00934    0.00855 =
         0.01001   -0.00020    0.00266   -0.00123
SE1   6    0.843904    0.446712    0.703870    11.00000    0.01042    0.00992 =
         0.01168   -0.00070    0.00284    0.00058
CL1   3    0.396933    0.543877    0.602929    11.00000    0.01027    0.01207 =
         0.01175   -0.00144    0.00464   -0.00137
CL2   3    0.480862    0.798319    0.428162    11.00000    0.01549    0.01219 =
         0.01591    0.00392    0.00276    0.00090
CL3   3    0.907060    0.695345    0.508586    11.00000    0.01220    0.01811 =
         0.01648    0.00038    0.00578   -0.00423
O1    5    0.700267    0.756851    0.705000    11.00000    0.01767    0.01397 =
         0.01434   -0.00291    0.00429   -0.00230
C2    1    1.055559    0.543795    0.797840    11.00000    0.01181    0.01818 =
         0.01664   -0.00207    0.00052   -0.00087
AFIX 137
H2A   2    1.021583    0.627519    0.831138    11.00000   -1.50000
H2B   2    1.129045    0.565762    0.744683    11.00000   -1.50000
H2C   2    1.120183    0.485869    0.863931    11.00000   -1.50000
AFIX   0
C1    1    0.732570    0.424411    0.838126    11.00000    0.01640    0.02088 =
         0.01533    0.00525    0.00643    0.00332
AFIX 137
H1A   2    0.804256    0.364995    0.900069    11.00000   -1.50000
H1B   2    0.617189    0.384192    0.806771    11.00000   -1.50000
H1C   2    0.721494    0.513073    0.873586    11.00000   -1.50000
AFIX   0
HKLF 4




REM  moocl3(seme)2-1_a.res in P2(1)/c
REM wR2 = 0.0354, GooF = S = 1.035, Restrained GooF = 1.035 for all data
REM R1 = 0.0167 for 2452 Fo > 4sig(Fo) and 0.0194 for all 2616 data
REM 75 parameters refined using 0 restraints

END  
     
WGHT      0.0120      0.6276 

REM Highest difference peak  0.637,  deepest hole -0.651,  1-sigma level  0.099
Q1    1   0.6506  0.6044  0.5378  11.00000  0.05    0.64
Q2    1   0.6768  0.7184  0.6367  11.00000  0.05    0.57
Q3    1   0.8466  0.3845  0.6645  11.00000  0.05    0.53
Q4    1   0.6538  0.7176  0.5373  11.00000  0.05    0.47
Q5    1   0.9714  0.4559  0.7336  11.00000  0.05    0.45
Q6    1   0.9120  0.3868  0.6840  11.00000  0.05    0.42
Q7    1   0.8150  0.4889  0.6511  11.00000  0.05    0.42
Q8    1   0.7507  0.4401  0.7861  11.00000  0.05    0.42
Q9    1   1.0643  0.4992  0.8700  11.00000  0.05    0.39
Q10   1   0.7584  0.6622  0.5012  11.00000  0.05    0.38
Q11   1   0.5168  0.5608  0.5857  11.00000  0.05    0.38
Q12   1   0.7663  0.4560  0.7113  11.00000  0.05    0.37
Q13   1   0.9563  0.4949  0.8042  11.00000  0.05    0.36
Q14   1   0.7439  0.6508  0.5790  11.00000  0.05    0.34
Q15   1   0.8300  0.7002  0.5269  11.00000  0.05    0.33
Q16   1   1.0559  0.6042  0.5522  11.00000  0.05    0.32
Q17   1   0.3527  0.5943  0.5397  11.00000  0.05    0.32
Q18   1   0.9388  0.7246  0.5836  11.00000  0.05    0.32
Q19   1   0.8483  0.7343  0.4147  11.00000  0.05    0.31
Q20   1   0.8639  0.5041  0.7524  11.00000  0.05    0.31

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0167 for 2452 Fo > 4sig(Fo) and 0.0194 for all 12252 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.64, deepest hole -0.65
  REM Mean Shift 0, Max Shift 0.001.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0194
  REM R1_gt = 0.0167
  REM wR_ref = 0.0354
  REM GOOF = 1.035
  REM Shift_max = 0.001
  REM Shift_mean = 0
  REM Reflections_all = 12252
  REM Reflections_gt = 2452
  REM Parameters = n/a
  REM Hole = -0.65
  REM Peak = 0.64
  REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.326
_oxdiff_exptl_absorpt_empirical_full_min 0.727
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
####################################################################### 
# 
# 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_moocl3(sme2)2-1
_database_code_depnum_ccdc_archive 'CCDC 2050672'
loop_
_audit_author_name
_audit_author_address
'Danielle Smith'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2020-12-16 deposited with the CCDC.	2021-02-26 downloaded from the CCDC.
;
_audit_creation_date             2020-05-04
_audit_creation_method           
;
Olex2 1.3
(compiled Sep 10 2019 10:52:38 for OlexSys, GUI svn.r5938)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[MoOCl2(SMe)2)(Cl)2]'
_chemical_formula_moiety         'C4 H12 Cl6 Mo2 O2 S2'
_chemical_formula_sum            'C4 H12 Cl6 Mo2 O2 S2'
_chemical_formula_weight         560.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         MoOCl3S2C4H12
_chemical_oxdiff_usercomment     'Dark Green Block'
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'
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'
O O 0.0106 0.0060 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   7.81110(10)
_cell_length_b                   9.50630(10)
_cell_length_c                   11.2487(2)
_cell_angle_alpha                90
_cell_angle_beta                 105.1720(10)
_cell_angle_gamma                90
_cell_volume                     806.15(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18670
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.7760
_cell_measurement_theta_min      2.8270
_shelx_estimated_absorpt_T_max   0.488
_shelx_estimated_absorpt_T_min   0.401
_exptl_absorpt_coefficient_mu    2.791
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.310
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_preparation       'Slow evporation from Toluene'
_exptl_crystal_recrystallization_method 'Slow evporation from Toluene'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_unetI/netI     0.0086
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21532
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.807
_diffrn_reflns_theta_min         3.754
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.9955
_diffrn_measured_fraction_theta_max 0.8997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -98.00  22.00   0.50    0.50    --   -8.30 -60.00-150.00  240
  2  ω    -98.00  22.00   0.50    0.50    --   -8.30 -60.00 -30.00  240
  3  ω    -98.00  21.00   0.50    0.50    --   -8.30 -57.00  60.00  238
  4  ω    -98.00  81.00   0.50    0.50    --   -8.30   0.00-180.00  358
  5  ω    -39.00  32.00   0.50    0.50    --   -8.30  60.00  30.00  142
  6  ω    -39.00  81.00   0.50    0.50    --   -8.30  60.00 -90.00  240
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0250907000
_diffrn_orient_matrix_UB_12      -0.0192916000
_diffrn_orient_matrix_UB_13      -0.0631257000
_diffrn_orient_matrix_UB_21      0.0900971000
_diffrn_orient_matrix_UB_22      0.0030738000
_diffrn_orient_matrix_UB_23      -0.0016747000
_diffrn_orient_matrix_UB_31      0.0105303000
_diffrn_orient_matrix_UB_32      -0.0719789000
_diffrn_orient_matrix_UB_33      0.0167839000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2654
_reflns_number_total             2693
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         2693
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0122
_refine_ls_R_factor_gt           0.0119
_refine_ls_restrained_S_all      1.208
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0094P)²+0.3552P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0276
_refine_ls_wR_factor_ref         0.0277
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.34606(2) 0.33611(2) 0.42055(2) 0.00912(3) Uani 1 1 d . . . . .
Cl3 Cl 0.60493(3) 0.45648(2) 0.39763(2) 0.01101(4) Uani 1 1 d . . . . .
Cl2 Cl 0.52835(3) 0.19600(3) 0.57247(2) 0.01500(5) Uani 1 1 d . . . . .
S1 S 0.16212(3) 0.53611(3) 0.29896(2) 0.01150(5) Uani 1 1 d . . . . .
Cl1 Cl 0.10043(3) 0.29556(3) 0.49632(2) 0.01515(5) Uani 1 1 d . . . . .
O1 O 0.30874(10) 0.23253(8) 0.29858(7) 0.01566(14) Uani 1 1 d . . . . .
C1 C -0.04121(13) 0.45007(12) 0.21690(10) 0.01628(19) Uani 1 1 d . . . . .
H1A H -0.106090 0.510654 0.152464 0.024 Uiso 1 1 calc R U . . .
H1B H -0.111970 0.430155 0.272964 0.024 Uiso 1 1 calc R U . . .
H1C H -0.013397 0.363770 0.181742 0.024 Uiso 1 1 calc R U . . .
C2 C 0.26029(14) 0.56851(12) 0.17281(10) 0.01639(19) Uani 1 1 d . . . . .
H2A H 0.273063 0.481098 0.133261 0.025 Uiso 1 1 calc R U . . .
H2B H 0.374747 0.611105 0.203770 0.025 Uiso 1 1 calc R U . . .
H2C H 0.185206 0.630526 0.114399 0.025 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 0.00845(4) 0.00929(4) 0.00973(4) -0.00034(3) 0.00260(3) -0.00124(2)
Cl3 0.00970(9) 0.01275(10) 0.01183(9) -0.00174(7) 0.00504(7) -0.00163(7)
Cl2 0.01483(10) 0.01318(10) 0.01606(11) 0.00366(8) 0.00239(8) 0.00103(8)
S1 0.01041(9) 0.01189(10) 0.01227(10) -0.00065(8) 0.00311(8) 0.00078(8)
Cl1 0.01162(10) 0.01954(11) 0.01530(10) 0.00028(9) 0.00536(8) -0.00502(8)
O1 0.0171(3) 0.0154(3) 0.0143(3) -0.0026(3) 0.0038(3) -0.0015(3)
C1 0.0103(4) 0.0188(5) 0.0182(5) -0.0008(4) 0.0010(3) -0.0006(3)
C2 0.0147(4) 0.0204(5) 0.0150(4) 0.0053(4) 0.0055(3) 0.0025(4)

_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 2.7942(2) 3_666 ?
Mo1 Cl3 2.3953(2) . ?
Mo1 Cl2 2.3341(3) . ?
Mo1 S1 2.5537(3) . ?
Mo1 Cl1 2.3264(2) . ?
Mo1 O1 1.6515(8) . ?
S1 C1 1.8100(10) . ?
S1 C2 1.8071(11) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?

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 Cl3 77.520(8) . 3_666 ?
Cl3 Mo1 S1 87.659(8) . . ?
Cl2 Mo1 Cl3 88.911(9) . . ?
Cl2 Mo1 Cl3 85.774(8) . 3_666 ?
Cl2 Mo1 S1 165.215(9) . . ?
S1 Mo1 Cl3 79.443(8) . 3_666 ?
Cl1 Mo1 Cl3 156.780(9) . . ?
Cl1 Mo1 Cl3 79.451(8) . 3_666 ?
Cl1 Mo1 Cl2 92.340(9) . . ?
Cl1 Mo1 S1 85.253(9) . . ?
O1 Mo1 Cl3 171.64(3) . 3_666 ?
O1 Mo1 Cl3 99.54(3) . . ?
O1 Mo1 Cl2 102.08(3) . . ?
O1 Mo1 S1 92.67(3) . . ?
O1 Mo1 Cl1 102.85(3) . . ?
Mo1 Cl3 Mo1 102.479(8) . 3_666 ?
C1 S1 Mo1 103.43(4) . . ?
C2 S1 Mo1 104.63(4) . . ?
C2 S1 C1 99.94(5) . . ?
S1 C1 H1A 109.5 . . ?
S1 C1 H1B 109.5 . . ?
S1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
S1 C2 H2A 109.5 . . ?
S1 C2 H2B 109.5 . . ?
S1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

_shelx_res_file                  
;
TITL moocl3(sme2)2-1_a.res in P2(1)/c
    moocl3(sme2)2-1.res
    created by SHELXL-2018/3 at 16:31:25 on 04-May-2020
REM Old TITL MoOCl3(SMe2)2-1 in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.032, Rweak 0.009, Alpha 0.022
REM <I/s> 3.892 for 108 systematic absences, Orientation as input
REM Formula found by SHELXT: C2 O S Cl3 Mo
CELL 0.71073 7.8111 9.5063 11.2487 90 105.172 90
ZERR 2 0.0001 0.0001 0.0002 0 0.001 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl Mo O S
UNIT 8 24 12 4 4 4

L.S. 4
PLAN  5
SIZE 0.4 0.3 0.3
BOND
list 4
fmap 2
acta
MORE -1
BOND $H
CONF
OMIT 2 0 2
REM <olex2.extras>
REM <HklSrc "%./MoOCl3(SMe2)2-1.hkl">
REM </olex2.extras>

WGHT    0.009400    0.355200
FVAR       0.62036
MO1   4    0.346060    0.336112    0.420554    11.00000    0.00845    0.00929 =
         0.00973   -0.00034    0.00260   -0.00124
CL3   3    0.604928    0.456476    0.397627    11.00000    0.00970    0.01275 =
         0.01183   -0.00174    0.00504   -0.00163
CL2   3    0.528355    0.195999    0.572471    11.00000    0.01483    0.01318 =
         0.01606    0.00366    0.00239    0.00103
S1    6    0.162121    0.536113    0.298958    11.00000    0.01041    0.01189 =
         0.01227   -0.00065    0.00311    0.00078
CL1   3    0.100426    0.295562    0.496318    11.00000    0.01162    0.01954 =
         0.01530    0.00028    0.00536   -0.00502
O1    5    0.308736    0.232535    0.298583    11.00000    0.01708    0.01545 =
         0.01428   -0.00261    0.00378   -0.00155
C1    1   -0.041205    0.450071    0.216898    11.00000    0.01032    0.01875 =
         0.01825   -0.00076    0.00104   -0.00058
AFIX 137
H1A   2   -0.106090    0.510654    0.152464    11.00000   -1.50000
H1B   2   -0.111970    0.430155    0.272964    11.00000   -1.50000
H1C   2   -0.013397    0.363770    0.181742    11.00000   -1.50000
AFIX   0
C2    1    0.260289    0.568507    0.172814    11.00000    0.01470    0.02037 =
         0.01502    0.00534    0.00554    0.00245
AFIX 137
H2A   2    0.273063    0.481098    0.133261    11.00000   -1.50000
H2B   2    0.374747    0.611105    0.203770    11.00000   -1.50000
H2C   2    0.185206    0.630526    0.114399    11.00000   -1.50000
AFIX   0
HKLF 4




REM  moocl3(sme2)2-1_a.res in P2(1)/c
REM wR2 = 0.0277, GooF = S = 1.208, Restrained GooF = 1.208 for all data
REM R1 = 0.0119 for 2654 Fo > 4sig(Fo) and 0.0122 for all 2693 data
REM 75 parameters refined using 0 restraints

END

WGHT      0.0094      0.3552

REM Highest difference peak  0.302,  deepest hole -0.483,  1-sigma level  0.064
Q1    1   0.2602  0.4474  0.3482  11.00000  0.05    0.30
Q2    1   0.2807  0.2487  0.3463  11.00000  0.05    0.29
Q3    1   0.3240  0.3103  0.3112  11.00000  0.05    0.26
Q4    1   0.2013  0.5462  0.2248  11.00000  0.05    0.24
Q5    1   0.5467  0.2760  0.5954  11.00000  0.05    0.23
;
_shelx_res_checksum              4806
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.727
_oxdiff_exptl_absorpt_empirical_full_min 0.609
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
####################################################################### 
# 
# 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_des_moocl3dithiahept-1
_database_code_depnum_ccdc_archive 'CCDC 2050674'
loop_
_audit_author_name
_audit_author_address
'Danielle Smith'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2020-12-16 deposited with the CCDC.	2021-02-26 downloaded from the CCDC.
;
_audit_creation_date             2020-12-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[MoOCl3(MeS(CH3)2SMe)]'
_chemical_formula_moiety         'C5 H12 Cl3 Mo O S2'
_chemical_formula_sum            'C5 H12 Cl3 Mo O S2'
_chemical_formula_weight         354.56
_chemical_melting_point          ?
_chemical_oxdiff_formula         MoOCl3C5H15S2
_chemical_oxdiff_usercomment     'Small green crystal'
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'
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'
O O 0.0106 0.0060 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.2795(2)
_cell_length_b                   12.7576(3)
_cell_length_c                   7.6118(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1192.44(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4060
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.6270
_cell_measurement_theta_min      3.5160
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.078
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.975
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_preparation       'Slow evporation from DCM'
_exptl_crystal_recrystallization_method 'Slow evporation from DCM'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6824
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.010
_diffrn_reflns_theta_min         3.116
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00  52.00   1.00    4.00    --  -15.60  38.00-150.00   96
  2  ω    -47.00  71.00   1.00    4.00    --  -15.60  57.00 120.00  118
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0304818000
_diffrn_orient_matrix_UB_12      -0.0305080000
_diffrn_orient_matrix_UB_13      -0.0603815000
_diffrn_orient_matrix_UB_21      0.0009210000
_diffrn_orient_matrix_UB_22      -0.0420640000
_diffrn_orient_matrix_UB_23      0.0609997000
_diffrn_orient_matrix_UB_31      -0.0490734000
_diffrn_orient_matrix_UB_32      -0.0197022000
_diffrn_orient_matrix_UB_33      -0.0363339000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1624
_reflns_number_total             1807
_reflns_odcompleteness_completeness 99.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1807
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0290
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0253P)²+0.7877P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0605
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C3(H3a,H3b)
2.b Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.64916(2) 0.250000 0.56850(3) 0.01072(8) Uani 1 2 d S T P . .
S1 S 0.72167(4) 0.40018(5) 0.75367(7) 0.01408(12) Uani 1 1 d . . . . .
Cl2 Cl 0.84405(5) 0.250000 0.49621(10) 0.01580(16) Uani 1 2 d S T P . .
Cl1 Cl 0.60486(4) 0.11716(5) 0.36758(7) 0.01863(13) Uani 1 1 d . . . . .
O1 O 0.54027(16) 0.250000 0.7005(3) 0.0174(5) Uani 1 2 d S T P . .
C2 C 0.80119(17) 0.35055(19) 0.9372(3) 0.0162(5) Uani 1 1 d . . . . .
H2A H 0.875138 0.339628 0.896247 0.019 Uiso 1 1 calc R . . . .
H2B H 0.803886 0.404883 1.026193 0.019 Uiso 1 1 calc R . . . .
C3 C 0.7634(2) 0.250000 1.0250(4) 0.0159(6) Uani 1 2 d S T P . .
H3A H 0.789066 0.250000 1.145538 0.019 Uiso 1 2 calc RS T P . .
H3B H 0.684409 0.249999 1.028325 0.019 Uiso 1 2 calc RS T P . .
C1 C 0.60456(19) 0.4519(2) 0.8666(3) 0.0229(5) Uani 1 1 d . . . . .
H1A H 0.551597 0.474828 0.782175 0.034 Uiso 1 1 calc GR . . . .
H1B H 0.626282 0.510091 0.938404 0.034 Uiso 1 1 calc GR . . . .
H1C H 0.573365 0.398264 0.939389 0.034 Uiso 1 1 calc GR . . . .

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 0.01196(12) 0.00847(15) 0.01173(13) 0.000 -0.00055(9) 0.000
S1 0.0186(2) 0.0090(3) 0.0147(2) -0.0007(2) -0.00184(19) 0.0001(2)
Cl2 0.0132(3) 0.0191(4) 0.0151(3) 0.000 0.0011(3) 0.000
Cl1 0.0249(3) 0.0128(3) 0.0182(2) -0.0033(2) -0.0045(2) -0.0023(2)
O1 0.0154(10) 0.0167(13) 0.0201(11) 0.000 0.0010(9) 0.000
C2 0.0196(10) 0.0114(12) 0.0176(10) -0.0028(9) -0.0058(8) 0.0007(9)
C3 0.0209(14) 0.0122(17) 0.0147(13) 0.000 -0.0026(12) 0.000
C1 0.0243(11) 0.0189(14) 0.0254(12) -0.0080(11) -0.0019(10) 0.0099(10)

_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 S1 2.5397(6) 7_565 ?
Mo1 S1 2.5397(6) . ?
Mo1 Cl2 2.4555(7) . ?
Mo1 Cl1 2.3467(6) 7_565 ?
Mo1 Cl1 2.3467(6) . ?
Mo1 O1 1.673(2) . ?
S1 C2 1.818(2) . ?
S1 C1 1.800(2) . ?
C2 C3 1.519(3) . ?

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
S1 Mo1 S1 97.94(3) 7_565 . ?
Cl2 Mo1 S1 77.449(17) . . ?
Cl2 Mo1 S1 77.449(17) . 7_565 ?
Cl1 Mo1 S1 84.153(19) . 7_565 ?
Cl1 Mo1 S1 171.02(2) . . ?
Cl1 Mo1 S1 171.02(2) 7_565 7_565 ?
Cl1 Mo1 S1 84.152(19) 7_565 . ?
Cl1 Mo1 Cl2 94.581(19) . . ?
Cl1 Mo1 Cl2 94.581(19) 7_565 . ?
Cl1 Mo1 Cl1 92.47(3) . 7_565 ?
O1 Mo1 S1 86.95(5) . . ?
O1 Mo1 S1 86.96(5) . 7_565 ?
O1 Mo1 Cl2 156.03(8) . . ?
O1 Mo1 Cl1 101.90(5) . 7_565 ?
O1 Mo1 Cl1 101.90(5) . . ?
C2 S1 Mo1 110.60(8) . . ?
C1 S1 Mo1 105.14(9) . . ?
C1 S1 C2 100.94(11) . . ?
C3 C2 S1 117.91(17) . . ?
C2 C3 C2 115.2(3) 7_565 . ?

_iucr_refine_instructions_details 
;
TITL des_moocl3dithiahept-1_a.res in Pnma
    des_moocl3dithiahept-1.res
    created by SHELXL-2018/3 at 11:34:36 on 23-Nov-2020
REM Old TITL DES_MoOCl3dithiahept-1 in Pnma
REM SHELXT solution in Pnma: R1 0.054, Rweak 0.083, Alpha 0.023
REM <I/s> 0.887 for 158 systematic absences, Orientation as input
REM Formula found by SHELXT: C5 O S2 Cl3 Mo
CELL 0.71073 12.2795 12.7576 7.6118 90 90 90
ZERR 4 0.0002 0.0003 0.0002 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H Cl Mo O S
UNIT 20 48 12 4 4 8

L.S. 4 0 0
PLAN  20
BOND
list 4
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\DES_MoOCl3dithiahept-1.hkl">
REM </olex2.extras>

WGHT    0.025300    0.787700
FVAR       0.35939
MO1   4    0.649161    0.250000    0.568498    10.50000    0.01196    0.00847 =
         0.01173    0.00000   -0.00055    0.00000
S1    6    0.721669    0.400180    0.753669    11.00000    0.01859    0.00898 =
         0.01468   -0.00067   -0.00184    0.00007
CL2   3    0.844047    0.250000    0.496210    10.50000    0.01317    0.01913 =
         0.01511    0.00000    0.00107    0.00000
CL1   3    0.604865    0.117158    0.367585    11.00000    0.02493    0.01276 =
         0.01819   -0.00325   -0.00447   -0.00231
O1    5    0.540273    0.250000    0.700493    10.50000    0.01539    0.01666 =
         0.02011    0.00000    0.00101    0.00000
C2    1    0.801191    0.350548    0.937158    11.00000    0.01958    0.01138 =
         0.01762   -0.00281   -0.00585    0.00074
AFIX  23
H2A   2    0.875138    0.339628    0.896247    11.00000   -1.20000
H2B   2    0.803886    0.404883    1.026193    11.00000   -1.20000
AFIX   0
C3    1    0.763376    0.250000    1.025031    10.50000    0.02086    0.01216 =
         0.01471    0.00000   -0.00261    0.00000
AFIX  23
H3A   2    0.789066    0.250000    1.145538    10.50000   -1.20000
H3B   2    0.684409    0.249999    1.028325    10.50000   -1.20000
AFIX   0
C1    1    0.604562    0.451874    0.866587    11.00000    0.02430    0.01893 =
         0.02541   -0.00798   -0.00190    0.00986
AFIX 137
H1A   2    0.551597    0.474828    0.782175    11.00000   -1.50000
H1B   2    0.626282    0.510091    0.938404    11.00000   -1.50000
H1C   2    0.573365    0.398264    0.939389    11.00000   -1.50000
AFIX   0
HKLF 4




REM  des_moocl3dithiahept-1_a.res in Pnma
REM wR2 = 0.0605, GooF = S = 1.074, Restrained GooF = 1.074 for all data
REM R1 = 0.0290 for 1624 Fo > 4sig(Fo) and 0.0357 for all 1807 data
REM 62 parameters refined using 0 restraints

END  
     
WGHT      0.0253      0.7878 

REM Highest difference peak  0.686,  deepest hole -0.593,  1-sigma level  0.121
Q1    1   0.5634  0.2500  0.6176  10.50000  0.05    0.69
Q2    1   0.6425  0.1815  0.4572  11.00000  0.05    0.57
Q3    1   0.6049  0.2500  0.4868  10.50000  0.05    0.57
Q4    1   0.7665  0.3917  0.8342  11.00000  0.05    0.54
Q5    1   0.7013  0.2500  0.6612  10.50000  0.05    0.53
Q6    1   0.7445  0.2500  0.5251  10.50000  0.05    0.51
Q7    1   0.6585  0.2049  0.6960  11.00000  0.05    0.51
Q8    1   0.8354  0.2500  0.3768  10.50000  0.05    0.51
Q9    1   0.7544  0.2500  0.5644  10.50000  0.05    0.50
Q10   1   0.6829  0.2500  0.4916  10.50000  0.05    0.47
Q11   1   0.6064  0.1233  0.4711  11.00000  0.05    0.47
Q12   1   0.6782  0.1208  0.4142  11.00000  0.05    0.46
Q13   1   0.8216  0.2500  0.6128  10.50000  0.05    0.46
Q14   1   0.8874  0.2500  0.5802  10.50000  0.05    0.46
Q15   1   0.6148  0.2500  0.6941  10.50000  0.05    0.46
Q16   1   0.6796  0.4167  0.8386  11.00000  0.05    0.46
Q17   1   0.6021  0.3862  1.1385  11.00000  0.05    0.43
Q18   1   0.4916  0.2500  0.6295  10.50000  0.05    0.43
Q19   1   0.5407  0.2500  0.9391  10.50000  0.05    0.43
Q20   1   0.6469  0.2500  0.9227  10.50000  0.05    0.42

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0290 for 1624 Fo > 4sig(Fo) and 0.0357 for all 7322 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.69, deepest hole -0.59
  REM Mean Shift 0, Max Shift -0.001.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0357
  REM R1_gt = 0.0290
  REM wR_ref = 0.0605
  REM GOOF = 1.074
  REM Shift_max = -0.001
  REM Shift_mean = 0
  REM Reflections_all = 7322
  REM Reflections_gt = 1624
  REM Parameters = n/a
  REM Hole = -0.59
  REM Peak = 0.69
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.838
_oxdiff_exptl_absorpt_empirical_full_min 0.718
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
####################################################################### 
# 
# 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_moocl3(prs(ch2)2spr)-3
_database_code_depnum_ccdc_archive 'CCDC 2050671'
loop_
_audit_author_name
_audit_author_address
'Danielle Smith'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2020-12-16 deposited with the CCDC.	2021-02-26 downloaded from the CCDC.
;
_audit_creation_date             2020-06-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[MoOCl3(PrS(CH2)2SPr)]'
_chemical_formula_moiety         'C8 H18 Cl3 Mo O S2'
_chemical_formula_sum            'C8 H18 Cl3 Mo O S2'
_chemical_formula_weight         396.63
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Mo O S2 C H Cl'
_chemical_oxdiff_usercomment     DL-meth_DAC_Pr
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'
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'
O O 0.0106 0.0060 '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'

_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.
;
_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'
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                   12.4629(2)
_cell_length_b                   13.7526(2)
_cell_length_c                   17.5032(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3000.00(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    24989
_cell_measurement_temperature    112(17)
_cell_measurement_theta_max      31.0600
_cell_measurement_theta_min      3.1650
_shelx_estimated_absorpt_T_max   0.732
_shelx_estimated_absorpt_T_min   0.635
_exptl_absorpt_coefficient_mu    1.662
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_preparation       'Slow evporation from DCM'
_exptl_crystal_recrystallization_method 'Slow evporation from DCM'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24043
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.354
_diffrn_reflns_theta_min         3.183
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      112(17)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -35.00  77.00   1.00   23.72    --  -12.00  38.00 150.00  112
  2  ω   -101.00  17.00   1.00   23.72    --  -12.00 -60.00-120.00  118
  3  ω   -101.00  17.00   1.00   23.72    --  -12.00 -60.00  30.00  118
  4  ω   -101.00  17.00   1.00   23.72    --  -12.00 -60.00 150.00  118
  5  ω    -35.00  77.00   1.00   23.72    --  -12.00  38.00 -60.00  112
  6  ω    -41.00  77.00   1.00   23.72    --  -12.00  57.00  60.00  118
  7  ω    -41.00  77.00   1.00   23.72    --  -12.00  60.00 -30.00  118
  8  ω    -41.00 -16.00   1.00   23.72    --  -12.00  60.00 120.00   25
  9  ω    -41.00  77.00   1.00   23.72    --  -12.00  57.00-150.00  118
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0021395000
_diffrn_orient_matrix_UB_12      -0.0009707000
_diffrn_orient_matrix_UB_13      -0.0404783000
_diffrn_orient_matrix_UB_21      0.0008917000
_diffrn_orient_matrix_UB_22      -0.0515666000
_diffrn_orient_matrix_UB_23      0.0007431000
_diffrn_orient_matrix_UB_31      -0.0568754000
_diffrn_orient_matrix_UB_32      -0.0007727000
_diffrn_orient_matrix_UB_33      0.0014891000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3643
_reflns_number_total             4429
_reflns_odcompleteness_completeness 97.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.324
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         4429
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0461
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0492P)²+2.8238P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1074
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Mo01 Mo 0.70240(2) 0.49945(2) 0.63478(2) 0.01627(9) Uani 1 1 d . . . . .
Cl3 Cl 0.79603(5) 0.64535(5) 0.60986(5) 0.02254(17) Uani 1 1 d . . . . .
Cl1 Cl 0.60245(6) 0.37959(5) 0.69968(4) 0.02241(17) Uani 1 1 d . . . . .
S1 S 0.70695(5) 0.59355(5) 0.77852(4) 0.01808(16) Uani 1 1 d . . . . .
S2 S 0.52217(6) 0.58970(5) 0.63315(4) 0.01753(16) Uani 1 1 d . . . . .
Cl2 Cl 0.86372(6) 0.42530(5) 0.67015(5) 0.02610(18) Uani 1 1 d . . . . .
O1 O 0.67966(17) 0.46348(15) 0.54506(13) 0.0247(5) Uani 1 1 d . . . . .
C7 C 0.5340(2) 0.70059(19) 0.57479(18) 0.0198(6) Uani 1 1 d . . . . .
H7 H 0.595380 0.738949 0.592497 0.024 Uiso 1 1 calc R . . . .
C4 C 0.6003(2) 0.68080(19) 0.76429(18) 0.0213(6) Uani 1 1 d . . . . .
H4A H 0.581350 0.709600 0.813056 0.026 Uiso 1 1 calc R . . . .
H4B H 0.625617 0.732413 0.731119 0.026 Uiso 1 1 calc R . . . .
C5 C 0.5012(2) 0.6348(2) 0.72924(17) 0.0205(6) Uani 1 1 d . . . . .
H5A H 0.443904 0.682561 0.728334 0.025 Uiso 1 1 calc R . . . .
H5B H 0.478021 0.581353 0.761439 0.025 Uiso 1 1 calc R . . . .
C8 C 0.5533(3) 0.6680(2) 0.49332(19) 0.0268(7) Uani 1 1 d . . . . .
H8A H 0.620129 0.633556 0.490456 0.040 Uiso 1 1 calc GR . . . .
H8B H 0.555972 0.723868 0.460461 0.040 Uiso 1 1 calc GR . . . .
H8C H 0.495966 0.626026 0.477386 0.040 Uiso 1 1 calc GR . . . .
C1 C 0.7484(2) 0.4459(2) 0.87371(19) 0.0243(7) Uani 1 1 d . . . . .
H1A H 0.767759 0.409362 0.829043 0.036 Uiso 1 1 calc GR . . . .
H1B H 0.727127 0.402013 0.913609 0.036 Uiso 1 1 calc GR . . . .
H1C H 0.808861 0.483497 0.890462 0.036 Uiso 1 1 calc GR . . . .
C2 C 0.6552(3) 0.5138(2) 0.85467(18) 0.0204(6) Uani 1 1 d . . . . .
H2 H 0.595235 0.475479 0.834652 0.024 Uiso 1 1 calc R . . . .
C6 C 0.4320(3) 0.7609(2) 0.5819(2) 0.0301(7) Uani 1 1 d . . . . .
H6A H 0.371716 0.723037 0.565219 0.045 Uiso 1 1 calc GR . . . .
H6B H 0.438173 0.818048 0.550734 0.045 Uiso 1 1 calc GR . . . .
H6C H 0.421973 0.779599 0.634257 0.045 Uiso 1 1 calc GR . . . .
C3 C 0.6176(3) 0.5712(2) 0.9238(2) 0.0268(7) Uani 1 1 d . . . . .
H3A H 0.672288 0.616582 0.938662 0.040 Uiso 1 1 calc GR . . . .
H3B H 0.603530 0.527376 0.965349 0.040 Uiso 1 1 calc GR . . . .
H3C H 0.553124 0.605894 0.911241 0.040 Uiso 1 1 calc GR . . . .

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
Mo01 0.01364(15) 0.01012(13) 0.02506(17) -0.00138(8) 0.00193(9) 0.00022(8)
Cl3 0.0165(4) 0.0156(3) 0.0355(4) 0.0030(3) 0.0027(3) -0.0033(2)
Cl1 0.0248(4) 0.0119(3) 0.0306(4) 0.0006(3) 0.0014(3) -0.0047(3)
S1 0.0160(3) 0.0121(3) 0.0262(4) 0.0002(3) -0.0011(3) -0.0014(2)
S2 0.0129(3) 0.0122(3) 0.0274(4) -0.0002(2) -0.0003(3) -0.0002(2)
Cl2 0.0171(3) 0.0153(3) 0.0459(5) -0.0015(3) -0.0015(3) 0.0053(3)
O1 0.0253(11) 0.0230(10) 0.0257(12) -0.0033(9) 0.0022(9) -0.0022(9)
C7 0.0190(14) 0.0129(12) 0.0275(17) 0.0022(11) -0.0001(12) 0.0017(11)
C4 0.0270(15) 0.0107(11) 0.0261(16) 0.0004(11) 0.0004(12) 0.0054(11)
C5 0.0180(14) 0.0183(13) 0.0251(16) 0.0016(11) 0.0034(12) 0.0061(11)
C8 0.0317(18) 0.0198(14) 0.0291(18) 0.0006(12) -0.0008(14) 0.0011(13)
C1 0.0161(15) 0.0200(14) 0.0369(19) 0.0046(12) -0.0041(12) -0.0010(12)
C2 0.0139(15) 0.0183(13) 0.0291(17) 0.0024(11) -0.0023(12) -0.0035(11)
C6 0.0283(17) 0.0254(15) 0.037(2) 0.0055(13) -0.0010(14) 0.0135(13)
C3 0.0224(16) 0.0279(15) 0.0301(18) 0.0000(13) 0.0005(13) 0.0009(12)

_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
Mo01 Cl3 2.3618(7) . ?
Mo01 Cl1 2.3578(7) . ?
Mo01 S1 2.8299(8) . ?
Mo01 S2 2.5665(7) . ?
Mo01 Cl2 2.3378(7) . ?
Mo01 O1 1.670(2) . ?
S1 C4 1.808(3) . ?
S1 C2 1.842(3) . ?
S2 C7 1.841(3) . ?
S2 C5 1.812(3) . ?
C7 H7 0.9800 . ?
C7 C8 1.514(4) . ?
C7 C6 1.522(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.517(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C2 1.527(4) . ?
C2 H2 0.9800 . ?
C2 C3 1.520(4) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?

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 Mo01 S1 76.45(3) . . ?
Cl3 Mo01 S2 91.12(2) . . ?
Cl1 Mo01 Cl3 160.72(3) . . ?
Cl1 Mo01 S1 84.37(2) . . ?
Cl1 Mo01 S2 83.17(2) . . ?
S2 Mo01 S1 78.83(2) . . ?
Cl2 Mo01 Cl3 89.69(3) . . ?
Cl2 Mo01 Cl1 91.25(3) . . ?
Cl2 Mo01 S1 86.95(3) . . ?
Cl2 Mo01 S2 165.14(3) . . ?
O1 Mo01 Cl3 99.31(8) . . ?
O1 Mo01 Cl1 98.99(8) . . ?
O1 Mo01 S1 167.04(8) . . ?
O1 Mo01 S2 89.10(8) . . ?
O1 Mo01 Cl2 105.41(8) . . ?
C4 S1 Mo01 99.57(10) . . ?
C4 S1 C2 103.73(14) . . ?
C2 S1 Mo01 111.35(10) . . ?
C7 S2 Mo01 109.69(9) . . ?
C5 S2 Mo01 106.36(10) . . ?
C5 S2 C7 104.06(13) . . ?
S2 C7 H7 109.4 . . ?
C8 C7 S2 106.87(19) . . ?
C8 C7 H7 109.4 . . ?
C8 C7 C6 111.8(3) . . ?
C6 C7 S2 109.8(2) . . ?
C6 C7 H7 109.4 . . ?
S1 C4 H4A 109.2 . . ?
S1 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C5 C4 S1 112.18(18) . . ?
C5 C4 H4A 109.2 . . ?
C5 C4 H4B 109.2 . . ?
S2 C5 H5A 108.8 . . ?
S2 C5 H5B 108.8 . . ?
C4 C5 S2 113.6(2) . . ?
C4 C5 H5A 108.8 . . ?
C4 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
S1 C2 H2 109.2 . . ?
C1 C2 S1 104.8(2) . . ?
C1 C2 H2 109.2 . . ?
C3 C2 S1 112.1(2) . . ?
C3 C2 C1 112.3(3) . . ?
C3 C2 H2 109.2 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo01 S1 C4 C5 46.4(2) . . . . ?
Mo01 S1 C2 C1 79.5(2) . . . . ?
Mo01 S1 C2 C3 -158.47(19) . . . . ?
Mo01 S2 C7 C8 65.8(2) . . . . ?
Mo01 S2 C7 C6 -172.78(19) . . . . ?
Mo01 S2 C5 C4 44.4(2) . . . . ?
S1 C4 C5 S2 -65.1(3) . . . . ?
C7 S2 C5 C4 -71.4(2) . . . . ?
C4 S1 C2 C1 -174.3(2) . . . . ?
C4 S1 C2 C3 -52.3(2) . . . . ?
C5 S2 C7 C8 179.2(2) . . . . ?
C5 S2 C7 C6 -59.3(2) . . . . ?
C2 S1 C4 C5 -68.5(2) . . . . ?

_iucr_refine_instructions_details 
;
TITL moocl3(prs(ch2)2spr)-3_a.res in Pbca
    moocl3(prs(ch2)2spr)-3.res
    created by SHELXL-2018/3 at 11:13:04 on 12-Jun-2020
REM Old TITL MoOCl3(PrS(CH2)2SPr)-3 in Pbca
REM SHELXT solution in Pbca: R1 0.100, Rweak 0.032, Alpha 0.016
REM <I/s> 0.601 for 376 systematic absences, Orientation as input
REM Formula found by SHELXT: C8 O S2 Cl3 Mo
CELL 0.71073 12.4629 13.7526 17.5032 90 90 90
ZERR 8 0.0002 0.0002 0.0006 0 0 0
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 Cl Mo O S
UNIT 64 144 24 8 8 16

L.S. 4
PLAN  8
SIZE 0.2 0.3 0.2
CONF
list 4
MORE -1
BOND $H
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\MoOCl3(PrS(CH2)2SPr)-3.hkl">
REM </olex2.extras>

WGHT    0.049200    2.823800
FVAR       0.24078
MO01  4    0.702397    0.499445    0.634775    11.00000    0.01364    0.01012 =
         0.02506   -0.00138    0.00193    0.00022
CL3   3    0.796027    0.645352    0.609864    11.00000    0.01647    0.01564 =
         0.03550    0.00295    0.00273   -0.00327
CL1   3    0.602448    0.379589    0.699678    11.00000    0.02476    0.01187 =
         0.03060    0.00062    0.00141   -0.00465
S1    6    0.706950    0.593548    0.778520    11.00000    0.01597    0.01206 =
         0.02622    0.00018   -0.00106   -0.00136
S2    6    0.522166    0.589697    0.633147    11.00000    0.01293    0.01225 =
         0.02741   -0.00024   -0.00030   -0.00019
CL2   3    0.863724    0.425305    0.670146    11.00000    0.01705    0.01529 =
         0.04595   -0.00154   -0.00147    0.00528
O1    5    0.679660    0.463481    0.545064    11.00000    0.02535    0.02300 =
         0.02566   -0.00331    0.00223   -0.00221
C7    1    0.533951    0.700591    0.574794    11.00000    0.01901    0.01289 =
         0.02753    0.00216   -0.00010    0.00175
AFIX  13
H7    2    0.595380    0.738949    0.592497    11.00000   -1.20000
AFIX   0
C4    1    0.600253    0.680800    0.764292    11.00000    0.02700    0.01070 =
         0.02615    0.00037    0.00042    0.00540
AFIX  23
H4A   2    0.581350    0.709600    0.813056    11.00000   -1.20000
H4B   2    0.625617    0.732413    0.731119    11.00000   -1.20000
AFIX   0
C5    1    0.501155    0.634794    0.729241    11.00000    0.01803    0.01834 =
         0.02506    0.00163    0.00342    0.00608
AFIX  23
H5A   2    0.443904    0.682561    0.728334    11.00000   -1.20000
H5B   2    0.478021    0.581353    0.761439    11.00000   -1.20000
AFIX   0
C8    1    0.553272    0.668032    0.493322    11.00000    0.03166    0.01981 =
         0.02905    0.00059   -0.00081    0.00107
AFIX 137
H8A   2    0.620129    0.633556    0.490456    11.00000   -1.50000
H8B   2    0.555972    0.723868    0.460461    11.00000   -1.50000
H8C   2    0.495966    0.626026    0.477386    11.00000   -1.50000
AFIX   0
C1    1    0.748399    0.445865    0.873715    11.00000    0.01605    0.01997 =
         0.03693    0.00456   -0.00406   -0.00101
AFIX 137
H1A   2    0.767759    0.409362    0.829043    11.00000   -1.50000
H1B   2    0.727127    0.402013    0.913609    11.00000   -1.50000
H1C   2    0.808861    0.483497    0.890462    11.00000   -1.50000
AFIX   0
C2    1    0.655243    0.513839    0.854669    11.00000    0.01386    0.01825 =
         0.02913    0.00240   -0.00226   -0.00348
AFIX  13
H2    2    0.595235    0.475479    0.834652    11.00000   -1.20000
AFIX   0
C6    1    0.432048    0.760883    0.581908    11.00000    0.02832    0.02542 =
         0.03670    0.00555   -0.00099    0.01347
AFIX 137
H6A   2    0.371716    0.723037    0.565219    11.00000   -1.50000
H6B   2    0.438173    0.818048    0.550734    11.00000   -1.50000
H6C   2    0.421973    0.779599    0.634257    11.00000   -1.50000
AFIX   0
C3    1    0.617579    0.571203    0.923849    11.00000    0.02238    0.02785 =
         0.03015   -0.00002    0.00051    0.00094
AFIX 137
H3A   2    0.672288    0.616582    0.938662    11.00000   -1.50000
H3B   2    0.603530    0.527376    0.965349    11.00000   -1.50000
H3C   2    0.553124    0.605894    0.911241    11.00000   -1.50000
AFIX   0
HKLF 4




REM  moocl3(prs(ch2)2spr)-3_a.res in Pbca
REM wR2 = 0.1074, GooF = S = 1.073, Restrained GooF = 1.073 for all data
REM R1 = 0.0461 for 3643 Fo > 4sig(Fo) and 0.0600 for all 4429 data
REM 140 parameters refined using 0 restraints

END  
     
WGHT      0.0492      2.8240 

REM Highest difference peak  1.324,  deepest hole -0.680,  1-sigma level  0.146
Q1    1   0.6427  0.4979  0.6365  11.00000  0.05    1.32
Q2    1   0.7634  0.4986  0.6339  11.00000  0.05    1.30
Q3    1   0.7197  0.4809  0.6792  11.00000  0.05    0.93
Q4    1   0.6958  0.4699  0.5913  11.00000  0.05    0.81
Q5    1   0.5940  0.5768  0.6381  11.00000  0.05    0.62
Q6    1   0.8038  0.6432  0.5640  11.00000  0.05    0.61
Q7    1   0.8023  0.4375  0.6758  11.00000  0.05    0.60
Q8    1   0.6611  0.5019  0.5509  11.00000  0.05    0.60

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0461 for 3643 Fo > 4sig(Fo) and 0.0600 for all 25666 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.32, deepest hole -0.68
  REM Mean Shift 0, Max Shift -0.002.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0600
  REM R1_gt = 0.0461
  REM wR_ref = 0.1074
  REM GOOF = 1.073
  REM Shift_max = -0.002
  REM Shift_mean = 0
  REM Reflections_all = 25666
  REM Reflections_gt = 3643
  REM Parameters = n/a
  REM Hole = -0.68
  REM Peak = 1.32
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.509
_oxdiff_exptl_absorpt_empirical_full_min 0.532
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
####################################################################### 
# 
# 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_jp20-1
_database_code_depnum_ccdc_archive 'CCDC 2050891'
loop_
_audit_author_name
_audit_author_address
'Danielle Smith'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2020-12-17 deposited with the CCDC.	2021-02-26 downloaded from the CCDC.
;
_audit_creation_date             2020-06-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[MoOCl3(MeS(CH2)3SMe)]'
_chemical_formula_moiety         'C5 H12 Cl3 Mo O S2'
_chemical_formula_sum            'C5 H12 Cl3 Mo O S2'
_chemical_formula_weight         354.56
_chemical_melting_point          ?
_chemical_oxdiff_formula         MoOCl3C4H5P
_chemical_oxdiff_usercomment     'Green/Yellow Block Dichromic'
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'
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'
O O 0.0106 0.0060 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.2610(2)
_cell_length_b                   12.7705(2)
_cell_length_c                   7.60850(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1191.33(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13406
_cell_measurement_temperature    99.98(18)
_cell_measurement_theta_max      31.4210
_cell_measurement_theta_min      4.2490
_shelx_estimated_absorpt_T_max   0.681
_shelx_estimated_absorpt_T_min   0.574
_exptl_absorpt_coefficient_mu    2.080
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_preparation       'Slow evporation from DCM'
_exptl_crystal_recrystallization_method 'Slow evporation from DCM'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            18361
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.503
_diffrn_reflns_theta_min         3.151
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -72.00  17.00   1.00    1.00    --  -10.30 -60.00  30.00   89
  2  ω    -82.00   3.00   1.00    1.00    --  -10.30 -60.00-180.00   85
  3  ω    -65.00 -30.00   1.00    1.00    --  -10.30 -60.00   0.00   35
  4  ω    -98.00 -38.00   1.00    1.00    --  -10.30   0.00-180.00   60
  5  ω    -14.00  78.00   1.00    1.00    --  -10.30   0.00-180.00   92
  6  ω    -33.00  48.00   1.00    1.00    --  -10.30  57.00 -60.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0345891000
_diffrn_orient_matrix_UB_12      -0.0014842000
_diffrn_orient_matrix_UB_13      0.0444754000
_diffrn_orient_matrix_UB_21      0.0463652000
_diffrn_orient_matrix_UB_22      -0.0002376000
_diffrn_orient_matrix_UB_23      0.0332200000
_diffrn_orient_matrix_UB_31      -0.0004705000
_diffrn_orient_matrix_UB_32      0.0932566000
_diffrn_orient_matrix_UB_33      0.0008005000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1909
_reflns_number_total             1948
_reflns_odcompleteness_completeness 99.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1948
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0187
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0158P)²+0.9071P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0428
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.35063(2) 0.750000 0.43171(2) 0.00953(5) Uani 1 2 d S T P . .
S1 S 0.27808(3) 0.60002(2) 0.24649(4) 0.01313(7) Uani 1 1 d . . . . .
Cl1 Cl 0.15559(4) 0.750000 0.50414(6) 0.01522(9) Uani 1 2 d S T P . .
Cl2 Cl 0.39480(3) 0.88271(3) 0.63250(4) 0.01790(8) Uani 1 1 d . . . . .
O1 O 0.45990(12) 0.750000 0.29982(19) 0.0169(3) Uani 1 2 d S T P . .
C2 C 0.19873(12) 0.64945(11) 0.06300(17) 0.0151(3) Uani 1 1 d . . . . .
H2A H 0.196098 0.595159 -0.026058 0.018 Uiso 1 1 calc R . . . .
H2B H 0.124642 0.660430 0.103719 0.018 Uiso 1 1 calc R . . . .
C3 C 0.23693(17) 0.750000 -0.0249(2) 0.0165(4) Uani 1 2 d S T P . .
H3A H 0.316025 0.750000 -0.027588 0.020 Uiso 1 2 calc RS T P . .
H3B H 0.211518 0.750001 -0.145584 0.020 Uiso 1 2 calc RS T P . .
C1 C 0.39535(13) 0.54811(12) 0.1339(2) 0.0227(3) Uani 1 1 d . . . . .
H1A H 0.427102 0.601725 0.061711 0.034 Uiso 1 1 calc GR . . . .
H1B H 0.373451 0.490298 0.061334 0.034 Uiso 1 1 calc GR . . . .
H1C H 0.448044 0.524622 0.218449 0.034 Uiso 1 1 calc GR . . . .

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 0.00963(8) 0.00959(8) 0.00939(8) 0.000 -0.00039(5) 0.000
S1 0.01694(16) 0.01017(13) 0.01227(14) -0.00072(11) -0.00170(11) -0.00033(11)
Cl1 0.01121(19) 0.0213(2) 0.0132(2) 0.000 0.00100(15) 0.000
Cl2 0.02310(17) 0.01434(14) 0.01625(15) -0.00345(11) -0.00452(12) -0.00230(12)
O1 0.0130(6) 0.0185(6) 0.0191(7) 0.000 0.0023(5) 0.000
C2 0.0169(6) 0.0137(6) 0.0149(6) -0.0021(5) -0.0052(5) -0.0001(5)
C3 0.0221(10) 0.0166(8) 0.0109(8) 0.000 -0.0014(7) 0.000
C1 0.0221(7) 0.0211(7) 0.0249(7) -0.0087(6) -0.0025(6) 0.0096(6)

_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 S1 2.5388(3) . ?
Mo1 S1 2.5388(3) 7_575 ?
Mo1 Cl1 2.4540(5) . ?
Mo1 Cl2 2.3451(3) 7_575 ?
Mo1 Cl2 2.3451(3) . ?
Mo1 O1 1.6739(14) . ?
S1 C2 1.8149(13) . ?
S1 C1 1.8004(15) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.5215(17) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?

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
S1 Mo1 S1 97.946(15) . 7_575 ?
Cl1 Mo1 S1 77.480(11) . 7_575 ?
Cl1 Mo1 S1 77.481(11) . . ?
Cl2 Mo1 S1 84.106(11) 7_575 . ?
Cl2 Mo1 S1 171.013(14) . . ?
Cl2 Mo1 S1 171.013(14) 7_575 7_575 ?
Cl2 Mo1 S1 84.107(11) . 7_575 ?
Cl2 Mo1 Cl1 94.517(12) . . ?
Cl2 Mo1 Cl1 94.517(12) 7_575 . ?
Cl2 Mo1 Cl2 92.555(17) . 7_575 ?
O1 Mo1 S1 87.00(3) . 7_575 ?
O1 Mo1 S1 87.00(3) . . ?
O1 Mo1 Cl1 156.14(5) . . ?
O1 Mo1 Cl2 101.87(4) . . ?
O1 Mo1 Cl2 101.87(4) . 7_575 ?
C2 S1 Mo1 110.64(4) . . ?
C1 S1 Mo1 105.20(5) . . ?
C1 S1 C2 100.95(7) . . ?
S1 C2 H2A 107.9 . . ?
S1 C2 H2B 107.9 . . ?
H2A C2 H2B 107.2 . . ?
C3 C2 S1 117.80(11) . . ?
C3 C2 H2A 107.9 . . ?
C3 C2 H2B 107.9 . . ?
C2 C3 C2 115.12(16) 7_575 . ?
C2 C3 H3A 108.5 . . ?
C2 C3 H3A 108.5 7_575 . ?
C2 C3 H3B 108.5 7_575 . ?
C2 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
S1 C1 H1A 109.5 . . ?
S1 C1 H1B 109.5 . . ?
S1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 S1 C2 C3 36.54(12) . . . . ?
S1 C2 C3 C2 -84.45(18) . . . 7_575 ?
C1 S1 C2 C3 -74.45(13) . . . . ?

_iucr_refine_instructions_details 
;
TITL jp20-1_a.res in Pnma
    jp20-1.res
    created by SHELXL-2018/3 at 11:09:56 on 12-Jun-2020
REM Old TITL JP20 - 1 in Pna2(1)
REM SHELXT solution in Pnma: R1 0.044, Rweak 0.007, Alpha 0.030
REM <I/s> 2.424 for 162 systematic absences, Orientation a'=-a, b'=c, c'=b
REM Formula found by SHELXT: C5 O Cl5 Mo
CELL 0.71073 12.261 12.7705 7.6085 90 90 90
ZERR 4 0.0002 0.0002 0.0001 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H Cl Mo O S
UNIT 20 48 12 4 4 8

L.S. 4
PLAN  4
SIZE 0.2 0.3 0.3
BOND
LIST 4
MORE -1
BOND $H
CONF
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\JP20%20-%201.hkl">
REM </olex2.extras>

WGHT    0.015800    0.907100
FVAR       0.42708
MO1   4    0.350626    0.750000    0.431711    10.50000    0.00963    0.00959 =
         0.00939    0.00000   -0.00039    0.00000
S1    6    0.278080    0.600024    0.246488    11.00000    0.01694    0.01017 =
         0.01227   -0.00072   -0.00170   -0.00033
CL1   3    0.155593    0.750000    0.504137    10.50000    0.01121    0.02127 =
         0.01320    0.00000    0.00100    0.00000
CL2   3    0.394798    0.882711    0.632501    11.00000    0.02310    0.01434 =
         0.01625   -0.00345   -0.00452   -0.00230
O1    5    0.459898    0.750000    0.299820    10.50000    0.01305    0.01847 =
         0.01911    0.00000    0.00229    0.00000
C2    1    0.198734    0.649451    0.063000    11.00000    0.01690    0.01368 =
         0.01486   -0.00211   -0.00524   -0.00008
AFIX  23
H2A   2    0.196098    0.595159   -0.026058    11.00000   -1.20000
H2B   2    0.124642    0.660430    0.103719    11.00000   -1.20000
AFIX   0
C3    1    0.236931    0.750000   -0.024851    10.50000    0.02213    0.01659 =
         0.01092    0.00000   -0.00135    0.00000
AFIX  23
H3A   2    0.316025    0.750000   -0.027588    10.50000   -1.20000
H3B   2    0.211518    0.750001   -0.145584    10.50000   -1.20000
AFIX   0
C1    1    0.395355    0.548109    0.133851    11.00000    0.02205    0.02110 =
         0.02490   -0.00870   -0.00249    0.00964
AFIX 137
H1A   2    0.427102    0.601725    0.061711    11.00000   -1.50000
H1B   2    0.373451    0.490298    0.061334    11.00000   -1.50000
H1C   2    0.448044    0.524622    0.218449    11.00000   -1.50000
AFIX   0
HKLF 4




REM  jp20-1_a.res in Pnma
REM wR2 = 0.0428, GooF = S = 1.106, Restrained GooF = 1.106 for all data
REM R1 = 0.0187 for 1909 Fo > 4sig(Fo) and 0.0194 for all 1948 data
REM 62 parameters refined using 0 restraints

END  
     
WGHT      0.0158      0.9071 

REM Highest difference peak  0.375,  deepest hole -0.530,  1-sigma level  0.081
Q1    1   0.3599  0.7500  0.6800  10.50000  0.05    0.37
Q2    1   0.4577  0.7500  0.4219  10.50000  0.05    0.37
Q3    1   0.4039  0.7359  0.2890  11.00000  0.05    0.33
Q4    1   0.4986  0.7500  0.3360  10.50000  0.05    0.32

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0187 for 1909 Fo > 4sig(Fo) and 0.0194 for all 19612 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.37, deepest hole -0.53
  REM Mean Shift 0, Max Shift 0.001.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0194
  REM R1_gt = 0.0187
  REM wR_ref = 0.0428
  REM GOOF = 1.106
  REM Shift_max = 0.001
  REM Shift_mean = 0
  REM Reflections_all = 19612
  REM Reflections_gt = 1909
  REM Parameters = n/a
  REM Hole = -0.53
  REM Peak = 0.37
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.810
_oxdiff_exptl_absorpt_empirical_full_min 0.668
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
####################################################################### 
# 
# 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_moocl3(mese(ch2)2seme)-1
_database_code_depnum_ccdc_archive 'CCDC 2050670'
loop_
_audit_author_name
_audit_author_address
'Danielle Smith'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2020-12-16 deposited with the CCDC.	2021-02-26 downloaded from the CCDC.
;
_audit_creation_date             2020-06-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[MoOCl3(MeSe(CH2)2SeMe)]'
_chemical_formula_moiety         'C4 H10 Cl3 Mo O Se2'
_chemical_formula_sum            'C4 H10 Cl3 Mo O Se2'
_chemical_formula_weight         434.33
_chemical_melting_point          ?
_chemical_oxdiff_formula         MoOCl3Se2C4H10
_chemical_oxdiff_usercomment     'Large Dark Green Block'
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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.45509(5)
_cell_length_b                   12.18741(7)
_cell_length_c                   12.53334(8)
_cell_angle_alpha                90
_cell_angle_beta                 96.6596(6)
_cell_angle_gamma                90
_cell_volume                     1131.074(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    30571
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      31.3350
_cell_measurement_theta_min      3.2060
_shelx_estimated_absorpt_T_max   0.289
_shelx_estimated_absorpt_T_min   0.137
_exptl_absorpt_coefficient_mu    8.254
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.551
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             812
_exptl_crystal_preparation       'Slow evporation from DCM'
_exptl_crystal_recrystallization_method 'Slow evporation from DCM'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36105
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.512
_diffrn_reflns_theta_min         3.219
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      105(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  79.00   1.00    1.00    --  -10.20  38.00   0.00  111
  2  ω   -100.00  17.00   1.00    1.00    --  -10.20 -60.00  90.00  117
  3  ω   -100.00  17.00   1.00    1.00    --  -10.20 -60.00-120.00  117
  4  ω    -32.00  79.00   1.00    1.00    --  -10.20  38.00  60.00  111
  5  ω   -100.00  11.00   1.00    1.00    --  -10.20 -38.00-120.00  111
  6  ω    -38.00  79.00   1.00    1.00    --  -10.20  60.00 -90.00  117
  7  ω    -38.00  79.00   1.00    1.00    --  -10.20  60.00 120.00  117
  8  ω   -100.00  -5.00   1.00    1.00    --  -10.20 -38.00 -60.00   95
  9  ω    -32.00  79.00   1.00    1.00    --  -10.20  38.00-150.00  111
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0642871000
_diffrn_orient_matrix_UB_12      0.0404268000
_diffrn_orient_matrix_UB_13      0.0102286000
_diffrn_orient_matrix_UB_21      -0.0392197000
_diffrn_orient_matrix_UB_22      -0.0371668000
_diffrn_orient_matrix_UB_23      0.0341674000
_diffrn_orient_matrix_UB_31      0.0592192000
_diffrn_orient_matrix_UB_32      0.0192702000
_diffrn_orient_matrix_UB_33      0.0444270000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3483
_reflns_number_total             3593
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         3593
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0198
_refine_ls_restrained_S_all      1.162
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0171P)²+0.8709P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0466
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.51493(2) 0.79910(2) 0.39691(2) 0.01167(4) Uani 1 1 d . . . . .
Se1 Se 0.20049(2) 0.70887(2) 0.32316(2) 0.01305(5) Uani 1 1 d . . . . .
Se2 Se 0.63893(2) 0.59953(2) 0.30408(2) 0.01494(5) Uani 1 1 d . . . . .
Cl1 Cl 0.54499(6) 0.67732(4) 0.54382(3) 0.01794(9) Uani 1 1 d . . . . .
Cl3 Cl 0.82369(6) 0.84090(4) 0.42759(4) 0.01935(9) Uani 1 1 d . . . . .
Cl2 Cl 0.50187(6) 0.86638(4) 0.22032(3) 0.01734(9) Uani 1 1 d . . . . .
O1 O 0.40335(19) 0.90014(11) 0.45095(11) 0.0186(3) Uani 1 1 d . . . . .
C2 C 0.2635(2) 0.60756(15) 0.21277(15) 0.0155(3) Uani 1 1 d . . . . .
H2A H 0.156474 0.566318 0.185745 0.019 Uiso 1 1 calc R . . . .
H2B H 0.300305 0.649854 0.153474 0.019 Uiso 1 1 calc R . . . .
C1 C 0.1388(3) 0.60561(16) 0.43161(15) 0.0184(3) Uani 1 1 d . . . . .
H1A H 0.239744 0.558104 0.451878 0.028 Uiso 1 1 calc GR . . . .
H1B H 0.036597 0.562559 0.402916 0.028 Uiso 1 1 calc GR . . . .
H1C H 0.109653 0.645218 0.493521 0.028 Uiso 1 1 calc GR . . . .
C3 C 0.4125(2) 0.52753(14) 0.25058(16) 0.0168(3) Uani 1 1 d . . . . .
H3A H 0.433270 0.479652 0.191413 0.020 Uiso 1 1 calc R . . . .
H3B H 0.373570 0.482231 0.307228 0.020 Uiso 1 1 calc R . . . .
C4 C 0.7169(3) 0.63701(17) 0.16591(17) 0.0214(4) Uani 1 1 d . . . . .
H4A H 0.615529 0.663511 0.118675 0.032 Uiso 1 1 calc GR . . . .
H4B H 0.765650 0.573028 0.135139 0.032 Uiso 1 1 calc GR . . . .
H4C H 0.807859 0.692995 0.175661 0.032 Uiso 1 1 calc GR . . . .

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 0.01407(8) 0.01060(7) 0.01031(8) -0.00003(5) 0.00126(5) -0.00022(5)
Se1 0.01231(8) 0.01324(8) 0.01341(9) -0.00004(6) 0.00075(6) 0.00104(6)
Se2 0.01497(9) 0.01504(8) 0.01445(9) -0.00077(6) 0.00024(6) 0.00396(6)
Cl1 0.0227(2) 0.01816(18) 0.01222(19) 0.00405(15) -0.00136(16) -0.00137(16)
Cl3 0.01529(19) 0.0230(2) 0.0196(2) 0.00047(16) 0.00151(16) -0.00294(15)
Cl2 0.0228(2) 0.01625(18) 0.01311(19) 0.00406(15) 0.00286(16) 0.00174(15)
O1 0.0233(7) 0.0163(6) 0.0167(7) -0.0019(5) 0.0054(5) 0.0023(5)
C2 0.0172(8) 0.0163(8) 0.0131(8) -0.0021(6) 0.0014(6) -0.0009(6)
C1 0.0196(9) 0.0213(8) 0.0148(8) -0.0003(7) 0.0042(7) -0.0051(7)
C3 0.0189(8) 0.0125(7) 0.0197(9) -0.0006(6) 0.0055(7) -0.0012(6)
C4 0.0218(9) 0.0214(9) 0.0228(10) -0.0019(7) 0.0103(8) -0.0021(7)

_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 Se1 2.6564(2) . ?
Mo1 Se2 2.8937(2) . ?
Mo1 Cl1 2.3554(4) . ?
Mo1 Cl3 2.3453(5) . ?
Mo1 Cl2 2.3517(4) . ?
Mo1 O1 1.6726(13) . ?
Se1 C2 1.9518(18) . ?
Se1 C1 1.9462(19) . ?
Se2 C3 1.9511(18) . ?
Se2 C4 1.944(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.513(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?

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
Se1 Mo1 Se2 79.763(7) . . ?
Cl1 Mo1 Se1 90.645(13) . . ?
Cl1 Mo1 Se2 77.220(12) . . ?
Cl3 Mo1 Se1 163.076(14) . . ?
Cl3 Mo1 Se2 83.987(13) . . ?
Cl3 Mo1 Cl1 90.349(17) . . ?
Cl3 Mo1 Cl2 90.648(17) . . ?
Cl2 Mo1 Se1 83.009(13) . . ?
Cl2 Mo1 Se2 83.968(12) . . ?
Cl2 Mo1 Cl1 160.950(17) . . ?
O1 Mo1 Se1 89.17(5) . . ?
O1 Mo1 Se2 168.15(5) . . ?
O1 Mo1 Cl1 98.86(5) . . ?
O1 Mo1 Cl3 107.37(5) . . ?
O1 Mo1 Cl2 98.99(5) . . ?
C2 Se1 Mo1 103.50(5) . . ?
C1 Se1 Mo1 107.17(6) . . ?
C1 Se1 C2 100.47(8) . . ?
C3 Se2 Mo1 102.25(5) . . ?
C4 Se2 Mo1 107.65(6) . . ?
C4 Se2 C3 97.79(8) . . ?
Se1 C2 H2A 108.6 . . ?
Se1 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
C3 C2 Se1 114.47(13) . . ?
C3 C2 H2A 108.6 . . ?
C3 C2 H2B 108.6 . . ?
Se1 C1 H1A 109.5 . . ?
Se1 C1 H1B 109.5 . . ?
Se1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Se2 C3 H3A 109.0 . . ?
Se2 C3 H3B 109.0 . . ?
C2 C3 Se2 113.10(12) . . ?
C2 C3 H3A 109.0 . . ?
C2 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
Se2 C4 H4A 109.5 . . ?
Se2 C4 H4B 109.5 . . ?
Se2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Se1 C2 C3 Se2 -59.81(16) . . . . ?

_iucr_refine_instructions_details 
;
TITL moocl3(mese(ch2)2seme)-1_a.res in P2(1)/n
    moocl3(mese(ch2)2seme)-1.res
    created by SHELXL-2018/3 at 11:22:12 on 12-Jun-2020
REM Old TITL MoOCl3(MeSe(CH2)2SeMe)-1 in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.040, Rweak 0.005, Alpha 0.019
REM <I/s> 2.780 for 120 systematic absences, Orientation as input
REM Formula found by SHELXT: C4 O Cl3 Se2 Mo
CELL 0.71073 7.455093 12.187409 12.533337 90 96.6596 90
ZERR 4 0.000046 0.000065 0.00008 0 0.0006 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Cl Mo O Se
UNIT 16 40 12 4 4 8

L.S. 4 0 0
PLAN  5
SIZE 0.2 0.3 0.4
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\MoOCl3(MeSe(CH2)2SeMe)-1.hkl">
REM </olex2.extras>

WGHT    0.017100    0.870900
FVAR       0.37129
MO1   4    0.514930    0.799104    0.396911    11.00000    0.01407    0.01060 =
         0.01031   -0.00003    0.00126   -0.00022
SE1   6    0.200489    0.708865    0.323157    11.00000    0.01231    0.01324 =
         0.01341   -0.00004    0.00075    0.00104
SE2   6    0.638934    0.599535    0.304076    11.00000    0.01497    0.01504 =
         0.01445   -0.00077    0.00024    0.00396
CL1   3    0.544993    0.677316    0.543824    11.00000    0.02265    0.01816 =
         0.01222    0.00405   -0.00136   -0.00137
CL3   3    0.823692    0.840902    0.427592    11.00000    0.01529    0.02302 =
         0.01960    0.00047    0.00151   -0.00294
CL2   3    0.501868    0.866379    0.220316    11.00000    0.02285    0.01625 =
         0.01311    0.00406    0.00286    0.00174
O1    5    0.403350    0.900136    0.450948    11.00000    0.02333    0.01634 =
         0.01673   -0.00192    0.00539    0.00225
C2    1    0.263464    0.607557    0.212774    11.00000    0.01715    0.01631 =
         0.01308   -0.00206    0.00136   -0.00086
AFIX  23
H2A   2    0.156474    0.566318    0.185745    11.00000   -1.20000
H2B   2    0.300305    0.649854    0.153474    11.00000   -1.20000
AFIX   0
C1    1    0.138807    0.605605    0.431607    11.00000    0.01962    0.02127 =
         0.01479   -0.00032    0.00415   -0.00506
AFIX 137
H1A   2    0.239744    0.558104    0.451878    11.00000   -1.50000
H1B   2    0.036597    0.562559    0.402916    11.00000   -1.50000
H1C   2    0.109653    0.645218    0.493521    11.00000   -1.50000
AFIX   0
C3    1    0.412510    0.527526    0.250580    11.00000    0.01893    0.01246 =
         0.01971   -0.00061    0.00548   -0.00119
AFIX  23
H3A   2    0.433270    0.479652    0.191413    11.00000   -1.20000
H3B   2    0.373570    0.482231    0.307228    11.00000   -1.20000
AFIX   0
C4    1    0.716852    0.637009    0.165905    11.00000    0.02177    0.02138 =
         0.02277   -0.00187    0.01032   -0.00213
AFIX 137
H4A   2    0.615529    0.663511    0.118675    11.00000   -1.50000
H4B   2    0.765650    0.573028    0.135139    11.00000   -1.50000
H4C   2    0.807859    0.692995    0.175661    11.00000   -1.50000
AFIX   0
HKLF 4




REM  moocl3(mese(ch2)2seme)-1_a.res in P2(1)/n
REM wR2 = 0.0466, GooF = S = 1.162, Restrained GooF = 1.162 for all data
REM R1 = 0.0198 for 3483 Fo > 4sig(Fo) and 0.0209 for all 3593 data
REM 102 parameters refined using 0 restraints

END  
     
WGHT      0.0171      0.8709 

REM Highest difference peak  0.856,  deepest hole -0.964,  1-sigma level  0.118
Q1    1   0.6142  0.7928  0.3931  11.00000  0.05    0.86
Q2    1   0.2979  0.7138  0.3232  11.00000  0.05    0.74
Q3    1   0.2017  0.7635  0.3201  11.00000  0.05    0.60
Q4    1   0.2047  0.6600  0.3203  11.00000  0.05    0.54
Q5    1   0.5191  0.7448  0.4004  11.00000  0.05    0.53

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0198 for 3483 Fo > 4sig(Fo) and 0.0209 for all 36967 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.86, deepest hole -0.96
  REM Mean Shift 0, Max Shift -0.002.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0209
  REM R1_gt = 0.0198
  REM wR_ref = 0.0466
  REM GOOF = 1.162
  REM Shift_max = -0.002
  REM Shift_mean = 0
  REM Reflections_all = 36967
  REM Reflections_gt = 3483
  REM Parameters = n/a
  REM Hole = -0.96
  REM Peak = 0.86
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.992
_oxdiff_exptl_absorpt_empirical_full_min 0.666
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
####################################################################### 
# 
# 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_moocl3dppm-1
_database_code_depnum_ccdc_archive 'CCDC 2050673'
loop_
_audit_author_name
_audit_author_address
'Danielle Smith'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2020-12-16 deposited with the CCDC.	2021-02-26 downloaded from the CCDC.
;
_audit_creation_date             2020-06-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[MoOCl(dmpe)2)(O)(MoOCl4)'
_chemical_formula_moiety         'C12 H32 Cl5 Mo2 O2 P4'
_chemical_formula_sum            'C12 H32 Cl5 Mo2 O2 P4'
_chemical_formula_weight         701.38
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         MoOCl3P2C20H20
_chemical_oxdiff_usercomment     'Purple Block'
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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   14.84971(13)
_cell_length_b                   12.54652(11)
_cell_length_c                   13.80599(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2572.22(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    45695
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.7750
_cell_measurement_theta_min      2.1180
_shelx_estimated_absorpt_T_max   0.721
_shelx_estimated_absorpt_T_min   0.541
_exptl_absorpt_coefficient_mu    1.750
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1396
_exptl_crystal_preparation       'Slow evporation from DCM'
_exptl_crystal_recrystallization_method 'Slow evporation from DCM'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0096
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48479
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.733
_diffrn_reflns_theta_min         2.125
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -98.00  22.00   0.50    0.50    --   -8.30 -60.00 -90.00  240
  2  ω    -98.00  22.00   0.50    0.50    --   -8.30 -60.00  30.00  240
  3  ω    -98.00  21.00   0.50    0.50    --   -8.30 -57.00 120.00  238
  4  ω    -98.00  81.00   0.50    0.50    --   -8.30   0.00-120.00  358
  5  ω    -39.00  81.00   0.50    0.50    --   -8.30  38.00 -90.00  240
  6  ω    -38.00  81.00   0.50    0.50    --   -8.30  57.00  90.00  238
  7  ω    -39.00  81.00   0.50    0.50    --   -8.30  60.00-180.00  240
  8  ω    -38.00  81.00   0.50    0.50    --   -8.30  57.00   0.00  238
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0063518000
_diffrn_orient_matrix_UB_12      -0.0533636000
_diffrn_orient_matrix_UB_13      0.0155963000
_diffrn_orient_matrix_UB_21      0.0471740000
_diffrn_orient_matrix_UB_22      0.0086503000
_diffrn_orient_matrix_UB_23      0.0022397000
_diffrn_orient_matrix_UB_31      -0.0041757000
_diffrn_orient_matrix_UB_32      0.0165773000
_diffrn_orient_matrix_UB_33      0.0488705000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.859
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.872
_reflns_number_gt                4440
_reflns_number_total             4445
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details 
;
 Flack x determined using 2042 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         4445
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0095
_refine_ls_R_factor_gt           0.0095
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0126P)²+0.9388P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0245
_refine_ls_wR_factor_ref         0.0245
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.000000 -0.69627(2) -0.11467(2) 0.00626(3) Uani 1 2 d S T P . .
Mo2 Mo 0.000000 -0.92957(2) 0.09296(2) 0.00915(3) Uani 1 2 d S T P . .
Cl1 Cl 0.000000 -0.54794(4) -0.23760(3) 0.01211(8) Uani 1 2 d S T P . .
Cl4 Cl 0.000000 -0.78350(4) 0.20035(4) 0.01499(8) Uani 1 2 d S T P . .
Cl2 Cl 0.000000 -1.03889(4) -0.04662(4) 0.01724(9) Uani 1 2 d S T P . .
O2 O 0.000000 -1.02613(12) 0.17481(11) 0.0168(3) Uani 1 2 d S T P . .
Cl3 Cl 0.15850(2) -0.90713(3) 0.07571(2) 0.01474(6) Uani 1 1 d . . . . .
P1 P -0.12725(2) -0.75294(3) -0.22306(3) 0.00905(6) Uani 1 1 d . . . . .
P2 P -0.12639(2) -0.59049(3) -0.04095(2) 0.00923(6) Uani 1 1 d . . . . .
O1 O 0.000000 -0.79513(10) -0.03012(10) 0.0101(2) Uani 1 2 d S T P . .
C1 C -0.14304(9) -0.59997(11) 0.08879(11) 0.0152(2) Uani 1 1 d . . . . .
H1A H -0.146753 -0.673613 0.107248 0.023 Uiso 1 1 calc GR . . . .
H1B H -0.197885 -0.564304 0.106251 0.023 Uiso 1 1 calc GR . . . .
H1C H -0.093312 -0.567023 0.121615 0.023 Uiso 1 1 calc GR . . . .
C2 C -0.22374(9) -0.66458(11) -0.19903(10) 0.0141(2) Uani 1 1 d . . . . .
H2A H -0.215641 -0.597993 -0.233648 0.017 Uiso 1 1 calc R . . . .
H2B H -0.278519 -0.697845 -0.222507 0.017 Uiso 1 1 calc R . . . .
C3 C -0.23278(8) -0.64194(11) -0.09047(9) 0.0129(2) Uani 1 1 d . . . . .
H3A H -0.249215 -0.707000 -0.056876 0.016 Uiso 1 1 calc R . . . .
H3B H -0.280261 -0.590102 -0.080006 0.016 Uiso 1 1 calc R . . . .
C4 C -0.12080(9) -0.75026(11) -0.35446(10) 0.0146(2) Uani 1 1 d . . . . .
H4A H -0.094394 -0.684201 -0.375063 0.022 Uiso 1 1 calc GR . . . .
H4B H -0.180256 -0.756588 -0.381160 0.022 Uiso 1 1 calc GR . . . .
H4C H -0.084351 -0.808572 -0.376589 0.022 Uiso 1 1 calc GR . . . .
C5 C -0.16840(9) -0.88530(11) -0.19458(10) 0.0146(2) Uani 1 1 d . . . . .
H5A H -0.124364 -0.937266 -0.213582 0.022 Uiso 1 1 calc GR . . . .
H5B H -0.223581 -0.898050 -0.228908 0.022 Uiso 1 1 calc GR . . . .
H5C H -0.179053 -0.890675 -0.126171 0.022 Uiso 1 1 calc GR . . . .
C6 C -0.12904(9) -0.44795(11) -0.06369(11) 0.0156(3) Uani 1 1 d . . . . .
H6A H -0.077790 -0.414931 -0.033756 0.023 Uiso 1 1 calc GR . . . .
H6B H -0.183275 -0.418324 -0.037083 0.023 Uiso 1 1 calc GR . . . .
H6C H -0.127466 -0.435243 -0.132235 0.023 Uiso 1 1 calc GR . . . .

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 0.00530(5) 0.00741(6) 0.00607(6) 0.00039(5) 0.000 0.000
Mo2 0.00829(6) 0.01019(6) 0.00897(7) 0.00239(5) 0.000 0.000
Cl1 0.01389(18) 0.01089(17) 0.01154(19) 0.00363(15) 0.000 0.000
Cl4 0.01587(19) 0.0171(2) 0.0120(2) -0.00188(17) 0.000 0.000
Cl2 0.0208(2) 0.01457(19) 0.0164(2) -0.00358(16) 0.000 0.000
O2 0.0181(7) 0.0150(6) 0.0174(7) 0.0062(5) 0.000 0.000
Cl3 0.00820(12) 0.02112(14) 0.01490(15) 0.00096(11) -0.00026(10) 0.00180(10)
P1 0.00837(13) 0.01112(13) 0.00765(13) -0.00040(10) -0.00122(11) -0.00038(10)
P2 0.00694(12) 0.01084(13) 0.00992(14) -0.00163(11) -0.00042(10) 0.00121(10)
O1 0.0089(5) 0.0108(6) 0.0106(6) 0.0013(5) 0.000 0.000
C1 0.0137(5) 0.0212(6) 0.0108(6) -0.0025(5) 0.0001(5) 0.0038(4)
C2 0.0107(5) 0.0180(6) 0.0136(6) -0.0021(5) -0.0040(4) 0.0028(4)
C3 0.0081(5) 0.0167(6) 0.0140(6) -0.0025(4) -0.0003(4) 0.0003(4)
C4 0.0151(6) 0.0190(6) 0.0096(6) 0.0001(5) -0.0025(5) -0.0001(5)
C5 0.0152(6) 0.0142(5) 0.0142(6) -0.0005(5) 0.0002(5) -0.0046(4)
C6 0.0132(6) 0.0122(5) 0.0213(7) -0.0026(5) 0.0016(5) 0.0025(4)

_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 Cl1 2.5187(5) . ?
Mo1 P1 2.5131(3) 3 ?
Mo1 P1 2.5131(3) . ?
Mo1 P2 2.5139(3) . ?
Mo1 P2 2.5139(3) 3 ?
Mo1 O1 1.7032(13) . ?
Mo2 Cl4 2.3574(5) . ?
Mo2 Cl2 2.3652(5) . ?
Mo2 O2 1.6567(15) . ?
Mo2 Cl3 2.3824(3) 3 ?
Mo2 Cl3 2.3824(3) . ?
Mo2 O1 2.3942(13) . ?
P1 C2 1.8417(13) . ?
P1 C4 1.8170(14) . ?
P1 C5 1.8126(14) . ?
P2 C1 1.8122(15) . ?
P2 C3 1.8385(13) . ?
P2 C6 1.8162(15) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.5314(19) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?

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
P1 Mo1 Cl1 78.919(11) 3 . ?
P1 Mo1 Cl1 78.920(11) . . ?
P1 Mo1 P1 97.515(16) . 3 ?
P1 Mo1 P2 162.137(13) 3 . ?
P1 Mo1 P2 80.156(10) . . ?
P1 Mo1 P2 80.156(10) 3 3 ?
P1 Mo1 P2 162.139(13) . 3 ?
P2 Mo1 Cl1 83.263(11) . . ?
P2 Mo1 Cl1 83.264(11) 3 . ?
P2 Mo1 P2 96.592(15) 3 . ?
O1 Mo1 Cl1 179.10(5) . . ?
O1 Mo1 P1 101.66(3) . . ?
O1 Mo1 P1 101.66(3) . 3 ?
O1 Mo1 P2 96.14(3) . 3 ?
O1 Mo1 P2 96.14(3) . . ?
Cl4 Mo2 Cl2 164.416(19) . . ?
Cl4 Mo2 Cl3 88.338(9) . 3 ?
Cl4 Mo2 Cl3 88.338(9) . . ?
Cl4 Mo2 O1 84.18(4) . . ?
Cl2 Mo2 Cl3 89.261(9) . . ?
Cl2 Mo2 Cl3 89.260(9) . 3 ?
Cl2 Mo2 O1 80.23(4) . . ?
O2 Mo2 Cl4 98.02(5) . . ?
O2 Mo2 Cl2 97.57(6) . . ?
O2 Mo2 Cl3 98.894(9) . 3 ?
O2 Mo2 Cl3 98.893(9) . . ?
O2 Mo2 O1 177.80(7) . . ?
Cl3 Mo2 Cl3 162.192(17) . 3 ?
Cl3 Mo2 O1 81.131(9) . . ?
Cl3 Mo2 O1 81.129(9) 3 . ?
C2 P1 Mo1 107.90(4) . . ?
C4 P1 Mo1 123.34(5) . . ?
C4 P1 C2 102.11(6) . . ?
C5 P1 Mo1 112.55(5) . . ?
C5 P1 C2 104.49(7) . . ?
C5 P1 C4 104.56(7) . . ?
C1 P2 Mo1 117.87(4) . . ?
C1 P2 C3 103.13(6) . . ?
C1 P2 C6 103.44(7) . . ?
C3 P2 Mo1 107.80(4) . . ?
C6 P2 Mo1 117.78(5) . . ?
C6 P2 C3 105.24(6) . . ?
Mo1 O1 Mo2 178.05(8) . . ?
P2 C1 H1A 109.5 . . ?
P2 C1 H1B 109.5 . . ?
P2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C3 C2 P1 110.87(9) . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
P2 C3 H3A 109.5 . . ?
P2 C3 H3B 109.5 . . ?
C2 C3 P2 110.71(9) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
P1 C4 H4A 109.5 . . ?
P1 C4 H4B 109.5 . . ?
P1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
P1 C5 H5A 109.5 . . ?
P1 C5 H5B 109.5 . . ?
P1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
P2 C6 H6A 109.5 . . ?
P2 C6 H6B 109.5 . . ?
P2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 P1 C2 C3 -40.23(10) . . . . ?
Mo1 P2 C3 C2 -41.43(10) . . . . ?
P1 C2 C3 P2 53.80(12) . . . . ?
C1 P2 C3 C2 -166.81(9) . . . . ?
C4 P1 C2 C3 -171.53(10) . . . . ?
C5 P1 C2 C3 79.75(10) . . . . ?
C6 P2 C3 C2 85.07(10) . . . . ?

_iucr_refine_instructions_details 
;
TITL MoOCl3dppm - 1 in Cmc21 #36
    moocl3dppm-1.res
    created by SHELXL-2018/3 at 11:03:21 on 12-Jun-2020
REM reset to Cmc21 #36
CELL 0.71073 14.849711 12.546521 13.80599 90 90 90
ZERR 4 0.000127 0.000106 0.000131 0 0 0
LATT -7
SYMM -X,-Y,0.5+Z
SYMM -X,+Y,+Z
SYMM +X,-Y,0.5+Z
SFAC C H Cl Mo O P
UNIT 48 128 20 8 8 16

L.S. 4
PLAN  10
SIZE 0.4 0.3 0.2
BOND
MORE -1
BOND $H
CONF
fmap 2
acta
OMIT 2 0 0
OMIT 1 1 -1
OMIT 0 0 -2
OMIT 1 1 1
REM <olex2.extras>
REM <HklSrc "%.\\MoOCl3dppm%20-%201.hkl">
REM </olex2.extras>

WGHT    0.012600    0.938800
FVAR       2.54329
MO1   4    0.000000   -0.696274   -0.114667    10.50000    0.00530    0.00741 =
         0.00607    0.00039    0.00000    0.00000
MO2   4    0.000000   -0.929571    0.092957    10.50000    0.00829    0.01019 =
         0.00897    0.00239    0.00000    0.00000
CL1   3    0.000000   -0.547937   -0.237595    10.50000    0.01389    0.01089 =
         0.01154    0.00363    0.00000    0.00000
CL4   3    0.000000   -0.783497    0.200351    10.50000    0.01587    0.01708 =
         0.01204   -0.00188    0.00000    0.00000
CL2   3    0.000000   -1.038892   -0.046616    10.50000    0.02079    0.01457 =
         0.01635   -0.00358    0.00000    0.00000
O2    5    0.000000   -1.026127    0.174814    10.50000    0.01814    0.01498 =
         0.01736    0.00621    0.00000    0.00000
CL3   3    0.158500   -0.907133    0.075710    11.00000    0.00820    0.02112 =
         0.01490    0.00096   -0.00026    0.00180
P1    6   -0.127254   -0.752942   -0.223060    11.00000    0.00837    0.01112 =
         0.00765   -0.00040   -0.00122   -0.00038
P2    6   -0.126390   -0.590494   -0.040953    11.00000    0.00694    0.01084 =
         0.00992   -0.00163   -0.00042    0.00121
O1    5    0.000000   -0.795133   -0.030119    10.50000    0.00891    0.01084 =
         0.01059    0.00127    0.00000    0.00000
C1    1   -0.143043   -0.599973    0.088794    11.00000    0.01366    0.02116 =
         0.01079   -0.00252    0.00012    0.00375
AFIX 137
H1A   2   -0.146753   -0.673613    0.107248    11.00000   -1.50000
H1B   2   -0.197885   -0.564304    0.106251    11.00000   -1.50000
H1C   2   -0.093312   -0.567023    0.121615    11.00000   -1.50000
AFIX   0
C2    1   -0.223739   -0.664585   -0.199032    11.00000    0.01073    0.01796 =
         0.01364   -0.00212   -0.00398    0.00283
AFIX  23
H2A   2   -0.215641   -0.597993   -0.233648    11.00000   -1.20000
H2B   2   -0.278519   -0.697845   -0.222507    11.00000   -1.20000
AFIX   0
C3    1   -0.232784   -0.641939   -0.090466    11.00000    0.00814    0.01673 =
         0.01398   -0.00246   -0.00028    0.00027
AFIX  23
H3A   2   -0.249215   -0.707000   -0.056876    11.00000   -1.20000
H3B   2   -0.280261   -0.590102   -0.080006    11.00000   -1.20000
AFIX   0
C4    1   -0.120803   -0.750259   -0.354462    11.00000    0.01514    0.01898 =
         0.00957    0.00012   -0.00250   -0.00007
AFIX 137
H4A   2   -0.094394   -0.684201   -0.375063    11.00000   -1.50000
H4B   2   -0.180256   -0.756588   -0.381160    11.00000   -1.50000
H4C   2   -0.084351   -0.808572   -0.376589    11.00000   -1.50000
AFIX   0
C5    1   -0.168402   -0.885298   -0.194581    11.00000    0.01521    0.01425 =
         0.01421   -0.00049    0.00017   -0.00457
AFIX 137
H5A   2   -0.124364   -0.937266   -0.213582    11.00000   -1.50000
H5B   2   -0.223581   -0.898050   -0.228908    11.00000   -1.50000
H5C   2   -0.179053   -0.890675   -0.126171    11.00000   -1.50000
AFIX   0
C6    1   -0.129043   -0.447948   -0.063686    11.00000    0.01323    0.01222 =
         0.02129   -0.00262    0.00163    0.00252
AFIX 137
H6A   2   -0.077790   -0.414931   -0.033756    11.00000   -1.50000
H6B   2   -0.183275   -0.418324   -0.037083    11.00000   -1.50000
H6C   2   -0.127466   -0.435243   -0.132235    11.00000   -1.50000
AFIX   0
HKLF 4




REM  MoOCl3dppm - 1 in Cmc21 #36
REM wR2 = 0.0245, GooF = S = 1.103, Restrained GooF = 1.103 for all data
REM R1 = 0.0095 for 4440 Fo > 4sig(Fo) and 0.0095 for all 4445 data
REM 128 parameters refined using 1 restraints

END  
     
WGHT      0.0125      0.9543 

REM Highest difference peak  0.325,  deepest hole -0.353,  1-sigma level  0.043
Q1    1   0.0000 -0.6674 -0.0680  10.50000  0.05    0.32
Q2    1  -0.1231 -0.7534 -0.2875  11.00000  0.05    0.26
Q3    1   0.0000 -0.7355 -0.1639  10.50000  0.05    0.25
Q4    1  -0.1240 -0.5077 -0.0528  11.00000  0.05    0.21
Q5    1   0.0000 -0.8022 -0.0837  10.50000  0.05    0.21
Q6    1   0.0000 -0.6007 -0.1694  10.50000  0.05    0.20
Q7    1   0.0000 -0.9795  0.1445  10.50000  0.05    0.20
Q8    1   0.0000 -0.7800  0.1433  10.50000  0.05    0.20
Q9    1   0.0000 -1.0216  0.1246  10.50000  0.05    0.20
Q10   1   0.0000 -0.8998  0.0482  10.50000  0.05    0.20

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0095 for 4440 Fo > 4sig(Fo) and 0.0095 for all 49570 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.32, deepest hole -0.35
  REM Mean Shift 0, Max Shift 0.002.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0095
  REM R1_gt = 0.0095
  REM wR_ref = 0.0245
  REM GOOF = 1.103
  REM Shift_max = 0.002
  REM Shift_mean = 0
  REM Reflections_all = 49570
  REM Reflections_gt = 4440
  REM Parameters = n/a
  REM Hole = -0.35
  REM Peak = 0.32
  REM Flack = -0.020(6)

  
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.717
_oxdiff_exptl_absorpt_empirical_full_min 0.608
####################################################################### 
# 
# 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_moocl3dmpe
_database_code_depnum_ccdc_archive 'CCDC 2050668'
loop_
_audit_author_name
_audit_author_address
'Danielle Smith'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2020-12-16 deposited with the CCDC.	2021-02-26 downloaded from the CCDC.
;
_audit_creation_date             2020-05-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        MoOCl3(dmpe)
_chemical_formula_moiety         'C6 H16 Cl3 Mo O P2'
_chemical_formula_sum            'C6 H16 Cl3 Mo O P2'
_chemical_formula_weight         368.42
_chemical_melting_point          ?
_chemical_oxdiff_formula         MoOCl3P2C6H9
_chemical_oxdiff_usercomment     'Yellow Block'
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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.37160(10)
_cell_length_b                   29.8674(6)
_cell_length_c                   12.4489(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.989(2)
_cell_angle_gamma                90
_cell_volume                     2734.24(8)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    30241
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.8010
_cell_measurement_theta_min      2.1310
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.745
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_preparation       'Slow evporation from DCM'
_exptl_crystal_recrystallization_method 'Slow evporation from DCM'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.787
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24936
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.787
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.852
_diffrn_reflns_theta_min         2.133
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.787
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -98.00  21.32   0.38    1.07    --   -8.30 -60.00  30.00  314
  2  ω    -98.00  20.18   0.38    1.07    --   -8.30 -57.00 150.00  311
  3  ω    -98.00  21.32   0.38    1.07    --   -8.30 -60.00 -90.00  314
  4  ω    -98.00  80.22   0.38    1.07    --   -8.30   0.00   0.00  469
  5  ω    -39.00  43.08   0.38    1.07    --   -8.30  38.00  30.00  216
  6  ω    -38.00  80.18   0.38    1.07    --   -8.30  57.00 120.00  311
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0041237000
_diffrn_orient_matrix_UB_12      -0.0039418000
_diffrn_orient_matrix_UB_13      0.0559725000
_diffrn_orient_matrix_UB_21      0.0846703000
_diffrn_orient_matrix_UB_22      -0.0113518000
_diffrn_orient_matrix_UB_23      0.0010796000
_diffrn_orient_matrix_UB_31      0.0460551000
_diffrn_orient_matrix_UB_32      0.0204752000
_diffrn_orient_matrix_UB_33      0.0113462000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7053
_reflns_number_total             8018
_reflns_odcompleteness_completeness 96.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.853
_refine_diff_density_min         -1.381
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         8018
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0417
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0616P)²+4.7250P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1117
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00G(H00D,H00E), C00H(H00F,H00G), C00I(H00Q,H00R), C00J(H00S,H00T)
2.b Idealised Me refined as rotating group:
 C00F(H00A,H00B,H00C), C00K(H00U,H00V,H00W), C00L(H00H,H00I,H00J), C00M(H00K,
 H00L,H00M), C00N(H00X,H00Y,H), C00O(H00Z,HA,HB), C00P(H00,HC,HD), C00Q(H00N,
 H00O,H00P)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Mo2 Mo 0.53671(3) 0.56966(2) 0.27879(2) 0.01293(7) Uani 1 1 d . . . . .
Mo1 Mo 0.09766(3) 0.69929(2) 0.73630(2) 0.01385(7) Uani 1 1 d . . . . .
Cl5 Cl 0.67718(9) 0.51686(2) 0.15010(5) 0.01634(13) Uani 1 1 d . . . . .
Cl6 Cl 0.68363(9) 0.52869(3) 0.42237(6) 0.01923(14) Uani 1 1 d . . . . .
Cl3 Cl 0.37835(9) 0.65222(3) 0.73692(6) 0.02083(15) Uani 1 1 d . . . . .
P4 P 0.29901(9) 0.50918(2) 0.25203(6) 0.01238(13) Uani 1 1 d . . . . .
Cl4 Cl 0.77757(10) 0.62088(3) 0.24815(6) 0.02151(15) Uani 1 1 d . . . . .
P2 P 0.01628(9) 0.65108(2) 0.57342(6) 0.01377(14) Uani 1 1 d . . . . .
P3 P 0.36375(10) 0.59513(2) 0.10597(6) 0.01499(14) Uani 1 1 d . . . . .
Cl1 Cl 0.23636(10) 0.74178(3) 0.88172(6) 0.02577(16) Uani 1 1 d . . . . .
P1 P 0.28312(9) 0.73585(3) 0.59739(6) 0.01518(14) Uani 1 1 d . . . . .
Cl2 Cl -0.03565(11) 0.64350(3) 0.84279(7) 0.02632(17) Uani 1 1 d . . . . .
O2 O 0.3920(3) 0.60123(8) 0.34543(18) 0.0205(4) Uani 1 1 d . . . . .
O1 O -0.0755(3) 0.73342(8) 0.6967(2) 0.0216(4) Uani 1 1 d . . . . .
C00F C 0.1073(4) 0.51980(11) 0.3305(2) 0.0185(5) Uani 1 1 d . . . . .
H00A H 0.143969 0.516771 0.405675 0.028 Uiso 1 1 calc GR . . . .
H00B H 0.012418 0.498674 0.311182 0.028 Uiso 1 1 calc GR . . . .
H00C H 0.063205 0.549632 0.316521 0.028 Uiso 1 1 calc GR . . . .
C00G C 0.1658(4) 0.55855(11) 0.0766(3) 0.0201(6) Uani 1 1 d . . . . .
H00D H 0.063521 0.569916 0.113375 0.024 Uiso 1 1 calc R . . . .
H00E H 0.132554 0.558971 -0.000117 0.024 Uiso 1 1 calc R . . . .
C00H C 0.2055(4) 0.51039(10) 0.1126(2) 0.0167(5) Uani 1 1 d . . . . .
H00F H 0.291540 0.497005 0.066557 0.020 Uiso 1 1 calc R . . . .
H00G H 0.094200 0.492995 0.105702 0.020 Uiso 1 1 calc R . . . .
C00I C 0.1135(4) 0.67570(10) 0.4551(2) 0.0171(5) Uani 1 1 d . . . . .
H00Q H 0.125517 0.652715 0.400998 0.020 Uiso 1 1 calc R . . . .
H00R H 0.032160 0.698602 0.424431 0.020 Uiso 1 1 calc R . . . .
C00J C 0.3009(4) 0.69644(10) 0.4858(3) 0.0180(5) Uani 1 1 d . . . . .
H00S H 0.344473 0.711964 0.424155 0.022 Uiso 1 1 calc R . . . .
H00T H 0.387167 0.673003 0.506927 0.022 Uiso 1 1 calc R . . . .
C00K C -0.2272(4) 0.64976(11) 0.5431(3) 0.0203(6) Uani 1 1 d . . . . .
H00U H -0.285764 0.640012 0.605496 0.030 Uiso 1 1 calc GR . . . .
H00V H -0.255651 0.629381 0.484708 0.030 Uiso 1 1 calc GR . . . .
H00W H -0.269371 0.679199 0.522954 0.030 Uiso 1 1 calc GR . . . .
C00L C 0.4881(5) 0.59626(11) -0.0134(2) 0.0215(6) Uani 1 1 d . . . . .
H00H H 0.598549 0.612915 0.000675 0.032 Uiso 1 1 calc GR . . . .
H00I H 0.415280 0.610254 -0.070884 0.032 Uiso 1 1 calc GR . . . .
H00J H 0.516720 0.566195 -0.033637 0.032 Uiso 1 1 calc GR . . . .
C00M C 0.3677(4) 0.45213(10) 0.2815(2) 0.0185(5) Uani 1 1 d . . . . .
H00K H 0.475050 0.445294 0.245206 0.028 Uiso 1 1 calc GR . . . .
H00L H 0.271621 0.432094 0.257188 0.028 Uiso 1 1 calc GR . . . .
H00M H 0.392954 0.448705 0.357752 0.028 Uiso 1 1 calc GR . . . .
C00N C 0.5096(4) 0.75276(12) 0.6449(3) 0.0241(6) Uani 1 1 d . . . . .
H00X H 0.502638 0.777801 0.692816 0.036 Uiso 1 1 calc GR . . . .
H00Y H 0.576824 0.761185 0.584749 0.036 Uiso 1 1 calc GR . . . .
H H 0.569927 0.728295 0.682520 0.036 Uiso 1 1 calc GR . . . .
C00O C 0.0888(5) 0.59323(10) 0.5808(3) 0.0234(6) Uani 1 1 d . . . . .
H00Z H 0.216062 0.591463 0.569309 0.035 Uiso 1 1 calc GR . . . .
HA H 0.020815 0.576154 0.526526 0.035 Uiso 1 1 calc GR . . . .
HB H 0.068156 0.581379 0.650619 0.035 Uiso 1 1 calc GR . . . .
C00P C 0.1823(5) 0.78589(11) 0.5372(3) 0.0258(7) Uani 1 1 d . . . . .
H00 H 0.064340 0.778897 0.503790 0.039 Uiso 1 1 calc GR . . . .
HC H 0.258495 0.797183 0.483866 0.039 Uiso 1 1 calc GR . . . .
HD H 0.170420 0.808151 0.591857 0.039 Uiso 1 1 calc GR . . . .
C00Q C 0.2666(5) 0.65021(11) 0.1194(3) 0.0235(6) Uani 1 1 d . . . . .
H00N H 0.186533 0.650059 0.177049 0.035 Uiso 1 1 calc GR . . . .
H00O H 0.199363 0.658266 0.053430 0.035 Uiso 1 1 calc GR . . . .
H00P H 0.362143 0.671562 0.134932 0.035 Uiso 1 1 calc GR . . . .

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
Mo2 0.01336(11) 0.01242(13) 0.01315(12) -0.00186(8) 0.00196(8) -0.00080(8)
Mo1 0.01232(11) 0.01402(13) 0.01539(12) -0.00247(8) 0.00223(9) -0.00132(8)
Cl5 0.0177(3) 0.0164(3) 0.0153(3) -0.0022(2) 0.0039(2) 0.0024(2)
Cl6 0.0181(3) 0.0239(4) 0.0156(3) 0.0035(3) 0.0009(2) 0.0009(2)
Cl3 0.0184(3) 0.0212(4) 0.0228(3) 0.0044(3) 0.0006(3) 0.0057(2)
P4 0.0135(3) 0.0108(3) 0.0131(3) -0.0007(2) 0.0023(2) -0.0002(2)
Cl4 0.0212(3) 0.0186(4) 0.0250(3) 0.0002(3) 0.0032(3) -0.0068(3)
P2 0.0134(3) 0.0113(3) 0.0168(3) -0.0017(2) 0.0020(3) -0.0015(2)
P3 0.0192(3) 0.0109(3) 0.0151(3) 0.0004(3) 0.0027(3) 0.0013(2)
Cl1 0.0239(3) 0.0306(4) 0.0227(3) -0.0107(3) 0.0008(3) -0.0076(3)
P1 0.0128(3) 0.0129(3) 0.0200(3) -0.0007(3) 0.0026(3) -0.0019(2)
Cl2 0.0303(4) 0.0257(4) 0.0239(4) 0.0009(3) 0.0088(3) -0.0101(3)
O2 0.0220(10) 0.0175(11) 0.0225(10) -0.0066(8) 0.0044(8) 0.0020(8)
O1 0.0151(9) 0.0189(11) 0.0308(12) -0.0057(9) 0.0011(8) 0.0024(8)
C00F 0.0167(12) 0.0193(14) 0.0202(13) -0.0009(11) 0.0057(11) 0.0003(10)
C00G 0.0191(12) 0.0210(15) 0.0196(13) 0.0016(11) -0.0031(11) -0.0011(11)
C00H 0.0185(12) 0.0158(14) 0.0154(12) -0.0021(10) -0.0005(10) -0.0032(10)
C00I 0.0171(12) 0.0183(14) 0.0160(12) 0.0000(10) 0.0025(10) -0.0002(10)
C00J 0.0134(11) 0.0206(15) 0.0203(13) -0.0003(11) 0.0038(10) -0.0012(10)
C00K 0.0135(11) 0.0234(16) 0.0240(14) -0.0041(12) 0.0017(11) -0.0040(10)
C00L 0.0319(15) 0.0157(15) 0.0175(13) 0.0035(11) 0.0058(12) 0.0050(12)
C00M 0.0232(13) 0.0127(13) 0.0200(13) -0.0001(10) 0.0031(11) 0.0014(10)
C00N 0.0164(12) 0.0240(16) 0.0321(17) -0.0032(13) 0.0025(12) -0.0100(11)
C00O 0.0308(15) 0.0107(14) 0.0286(16) -0.0017(12) 0.0011(13) -0.0004(11)
C00P 0.0311(16) 0.0154(15) 0.0311(17) 0.0020(12) 0.0036(14) 0.0015(12)
C00Q 0.0290(15) 0.0150(15) 0.0265(15) 0.0016(12) 0.0027(13) 0.0060(12)

_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
Mo2 Cl5 2.5213(7) . ?
Mo2 Cl6 2.3655(7) . ?
Mo2 P4 2.5226(7) . ?
Mo2 Cl4 2.3942(7) . ?
Mo2 P3 2.5400(8) . ?
Mo2 O2 1.685(2) . ?
Mo1 Cl3 2.5011(7) . ?
Mo1 P2 2.5249(8) . ?
Mo1 Cl1 2.3825(8) . ?
Mo1 P1 2.5261(8) . ?
Mo1 Cl2 2.3835(8) . ?
Mo1 O1 1.680(2) . ?
P4 C00F 1.802(3) . ?
P4 C00H 1.823(3) . ?
P4 C00M 1.808(3) . ?
P2 C00I 1.836(3) . ?
P2 C00K 1.809(3) . ?
P2 C00O 1.809(3) . ?
P3 C00G 1.839(3) . ?
P3 C00L 1.800(3) . ?
P3 C00Q 1.807(3) . ?
P1 C00J 1.833(3) . ?
P1 C00N 1.804(3) . ?
P1 C00P 1.809(3) . ?
C00G C00H 1.528(4) . ?
C00I C00J 1.538(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
_geom_angle_publ_flag
Cl5 Mo2 P4 77.31(2) . . ?
Cl5 Mo2 P3 81.56(2) . . ?
Cl6 Mo2 Cl5 88.28(3) . . ?
Cl6 Mo2 P4 90.38(3) . . ?
Cl6 Mo2 Cl4 98.35(3) . . ?
Cl6 Mo2 P3 166.27(3) . . ?
P4 Mo2 P3 78.43(2) . . ?
Cl4 Mo2 Cl5 87.51(3) . . ?
Cl4 Mo2 P4 162.27(3) . . ?
Cl4 Mo2 P3 90.45(3) . . ?
O2 Mo2 Cl5 164.81(8) . . ?
O2 Mo2 Cl6 100.94(8) . . ?
O2 Mo2 P4 90.46(8) . . ?
O2 Mo2 Cl4 102.88(8) . . ?
O2 Mo2 P3 87.23(8) . . ?
Cl3 Mo1 P2 80.34(3) . . ?
Cl3 Mo1 P1 76.00(3) . . ?
P2 Mo1 P1 78.84(2) . . ?
Cl1 Mo1 Cl3 89.19(3) . . ?
Cl1 Mo1 P2 168.36(3) . . ?
Cl1 Mo1 P1 93.77(3) . . ?
Cl1 Mo1 Cl2 96.98(3) . . ?
Cl2 Mo1 Cl3 88.76(3) . . ?
Cl2 Mo1 P2 87.93(3) . . ?
Cl2 Mo1 P1 161.21(3) . . ?
O1 Mo1 Cl3 162.42(8) . . ?
O1 Mo1 P2 88.71(8) . . ?
O1 Mo1 Cl1 100.17(8) . . ?
O1 Mo1 P1 88.47(8) . . ?
O1 Mo1 Cl2 104.66(8) . . ?
C00F P4 Mo2 111.48(11) . . ?
C00F P4 C00H 104.72(14) . . ?
C00F P4 C00M 105.98(14) . . ?
C00H P4 Mo2 108.94(10) . . ?
C00M P4 Mo2 117.77(10) . . ?
C00M P4 C00H 107.10(14) . . ?
C00I P2 Mo1 109.38(10) . . ?
C00K P2 Mo1 110.91(11) . . ?
C00K P2 C00I 106.15(14) . . ?
C00K P2 C00O 105.99(16) . . ?
C00O P2 Mo1 116.79(12) . . ?
C00O P2 C00I 107.04(15) . . ?
C00G P3 Mo2 109.56(10) . . ?
C00L P3 Mo2 116.77(11) . . ?
C00L P3 C00G 106.84(15) . . ?
C00L P3 C00Q 106.71(15) . . ?
C00Q P3 Mo2 111.91(12) . . ?
C00Q P3 C00G 104.19(15) . . ?
C00J P1 Mo1 108.18(10) . . ?
C00N P1 Mo1 115.40(12) . . ?
C00N P1 C00J 108.38(15) . . ?
C00N P1 C00P 104.42(17) . . ?
C00P P1 Mo1 114.50(12) . . ?
C00P P1 C00J 105.39(16) . . ?
C00H C00G P3 111.6(2) . . ?
C00G C00H P4 110.5(2) . . ?
C00J C00I P2 110.9(2) . . ?
C00I C00J P1 109.68(19) . . ?

_iucr_refine_instructions_details 
;
TITL moocl3dmpe_a.res in P2(1)/n
    moocl3dmpe.res
    created by SHELXL-2018/3 at 15:16:37 on 10-May-2020
REM Old TITL MoOCl3dmpe in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.070, Rweak 0.004, Alpha 0.049
REM <I/s> 0.539 for 122 systematic absences, Orientation as input
REM Formula found by SHELXT: C12 O2 Cl10 Mo2
CELL 0.71073 7.3716 29.8674 12.4489 90 93.989 90
ZERR 8 0.0001 0.0006 0.0002 0 0.002 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Cl Mo O P
UNIT 48 128 24 8 8 16

L.S. 4
PLAN  20
BOND
list 4
fmap 2
ACTA
OMIT 0 1 1
REM <olex2.extras>
REM <HklSrc "%.\\MoOCl3dmpe.hkl">
REM </olex2.extras>

WGHT    0.061600    4.725000
FVAR       0.25659
MO2   4    0.536715    0.569659    0.278794    11.00000    0.01336    0.01242 =
         0.01315   -0.00186    0.00196   -0.00080
MO1   4    0.097659    0.699285    0.736303    11.00000    0.01232    0.01402 =
         0.01539   -0.00247    0.00223   -0.00132
CL5   3    0.677183    0.516856    0.150096    11.00000    0.01770    0.01637 =
         0.01535   -0.00221    0.00394    0.00245
CL6   3    0.683633    0.528693    0.422370    11.00000    0.01813    0.02390 =
         0.01561    0.00354    0.00088    0.00092
CL3   3    0.378355    0.652219    0.736916    11.00000    0.01842    0.02119 =
         0.02277    0.00437    0.00059    0.00575
P4    6    0.299008    0.509176    0.252029    11.00000    0.01346    0.01079 =
         0.01308   -0.00072    0.00228   -0.00018
CL4   3    0.777567    0.620876    0.248154    11.00000    0.02120    0.01861 =
         0.02495    0.00024    0.00319   -0.00676
P2    6    0.016282    0.651080    0.573420    11.00000    0.01337    0.01129 =
         0.01678   -0.00167    0.00196   -0.00154
P3    6    0.363745    0.595134    0.105971    11.00000    0.01918    0.01086 =
         0.01512    0.00039    0.00266    0.00129
CL1   3    0.236357    0.741783    0.881725    11.00000    0.02391    0.03058 =
         0.02271   -0.01073    0.00083   -0.00757
P1    6    0.283116    0.735849    0.597389    11.00000    0.01281    0.01291 =
         0.02004   -0.00075    0.00263   -0.00187
CL2   3   -0.035649    0.643497    0.842795    11.00000    0.03032    0.02572 =
         0.02388    0.00093    0.00884   -0.01015
O2    5    0.391992    0.601228    0.345434    11.00000    0.02199    0.01753 =
         0.02250   -0.00660    0.00443    0.00198
O1    5   -0.075465    0.733420    0.696745    11.00000    0.01506    0.01893 =
         0.03076   -0.00568    0.00112    0.00240
C00F  1    0.107257    0.519805    0.330518    11.00000    0.01674    0.01927 =
         0.02018   -0.00086    0.00570    0.00025
AFIX 137
H00A  2    0.143969    0.516771    0.405675    11.00000   -1.50000
H00B  2    0.012418    0.498674    0.311182    11.00000   -1.50000
H00C  2    0.063205    0.549632    0.316521    11.00000   -1.50000
AFIX   0
C00G  1    0.165818    0.558551    0.076646    11.00000    0.01909    0.02097 =
         0.01965    0.00160   -0.00308   -0.00109
AFIX  23
H00D  2    0.063521    0.569916    0.113375    11.00000   -1.20000
H00E  2    0.132554    0.558971   -0.000117    11.00000   -1.20000
AFIX   0
C00H  1    0.205509    0.510395    0.112579    11.00000    0.01855    0.01581 =
         0.01538   -0.00212   -0.00046   -0.00322
AFIX  23
H00F  2    0.291540    0.497005    0.066557    11.00000   -1.20000
H00G  2    0.094200    0.492995    0.105702    11.00000   -1.20000
AFIX   0

C00I  1    0.113451    0.675699    0.455089    11.00000    0.01711    0.01833 =
         0.01598    0.00004    0.00254   -0.00017
AFIX  23
H00Q  2    0.125517    0.652715    0.400998    11.00000   -1.20000
H00R  2    0.032160    0.698602    0.424431    11.00000   -1.20000
AFIX   0
C00J  1    0.300860    0.696441    0.485766    11.00000    0.01344    0.02060 =
         0.02030   -0.00028    0.00384   -0.00117
AFIX  23
H00S  2    0.344473    0.711964    0.424155    11.00000   -1.20000
H00T  2    0.387167    0.673003    0.506927    11.00000   -1.20000
AFIX   0
C00K  1   -0.227184    0.649764    0.543086    11.00000    0.01351    0.02341 =
         0.02398   -0.00411    0.00168   -0.00398
AFIX 137
H00U  2   -0.285764    0.640012    0.605496    11.00000   -1.50000
H00V  2   -0.255651    0.629381    0.484708    11.00000   -1.50000
H00W  2   -0.269371    0.679199    0.522954    11.00000   -1.50000
AFIX   0

C00L  1    0.488075    0.596256   -0.013391    11.00000    0.03191    0.01573 =
         0.01754    0.00349    0.00580    0.00503
AFIX 137
H00H  2    0.598549    0.612915    0.000675    11.00000   -1.50000
H00I  2    0.415280    0.610254   -0.070884    11.00000   -1.50000
H00J  2    0.516720    0.566195   -0.033637    11.00000   -1.50000
AFIX   0
C00M  1    0.367714    0.452129    0.281499    11.00000    0.02316    0.01266 =
         0.01997   -0.00010    0.00308    0.00140
AFIX 137
H00K  2    0.475050    0.445294    0.245206    11.00000   -1.50000
H00L  2    0.271621    0.432094    0.257188    11.00000   -1.50000
H00M  2    0.392954    0.448705    0.357752    11.00000   -1.50000
AFIX   0

C00N  1    0.509627    0.752761    0.644930    11.00000    0.01637    0.02395 =
         0.03207   -0.00319    0.00248   -0.00998
AFIX 137
H00X  2    0.502638    0.777801    0.692816    11.00000   -1.50000
H00Y  2    0.576824    0.761185    0.584749    11.00000   -1.50000
H     2    0.569927    0.728295    0.682520    11.00000   -1.50000
AFIX   0
C00O  1    0.088843    0.593231    0.580839    11.00000    0.03077    0.01071 =
         0.02864   -0.00174    0.00109   -0.00036
AFIX 137
H00Z  2    0.216062    0.591463    0.569309    11.00000   -1.50000
HA    2    0.020815    0.576154    0.526526    11.00000   -1.50000
HB    2    0.068156    0.581379    0.650619    11.00000   -1.50000
AFIX   0
C00P  1    0.182262    0.785890    0.537161    11.00000    0.03113    0.01538 =
         0.03107    0.00196    0.00364    0.00152
AFIX 137
H00   2    0.064340    0.778897    0.503790    11.00000   -1.50000
HC    2    0.258495    0.797183    0.483866    11.00000   -1.50000
HD    2    0.170420    0.808151    0.591857    11.00000   -1.50000
AFIX   0

C00Q  1    0.266561    0.650207    0.119421    11.00000    0.02904    0.01501 =
         0.02645    0.00161    0.00268    0.00600
AFIX 137
H00N  2    0.186533    0.650059    0.177049    11.00000   -1.50000
H00O  2    0.199363    0.658266    0.053430    11.00000   -1.50000
H00P  2    0.362143    0.671562    0.134932    11.00000   -1.50000
AFIX   0
HKLF 4




REM  moocl3dmpe_a.res in P2(1)/n
REM wR2 = 0.1117, GooF = S = 1.029, Restrained GooF = 1.029 for all data
REM R1 = 0.0417 for 7053 Fo > 4sig(Fo) and 0.0486 for all 8018 data
REM 243 parameters refined using 0 restraints

END  
     
WGHT      0.0616      4.7170 

REM Highest difference peak  3.853,  deepest hole -1.381,  1-sigma level  0.169
Q1    1   0.6087  0.5516  0.3018  11.00000  0.05    3.85
Q2    1   0.5738  0.5683  0.2238  11.00000  0.05    2.08
Q3    1   0.0632  0.6984  0.7933  11.00000  0.05    1.95
Q4    1   0.5021  0.5693  0.3385  11.00000  0.05    1.89
Q5    1   0.1390  0.6998  0.6789  11.00000  0.05    1.76
Q6    1   0.8343  0.6092  0.2967  11.00000  0.05    1.51
Q7    1   0.4400  0.5906  0.4267  11.00000  0.05    1.41
Q8    1   0.1851  0.6825  0.7660  11.00000  0.05    1.17
Q9    1   0.4435  0.5871  0.1889  11.00000  0.05    1.13
Q10   1   0.4255  0.5951  0.0529  11.00000  0.05    1.04
Q11   1  -0.0081  0.7143  0.6766  11.00000  0.05    1.01
Q12   1   0.1867  0.7159  0.7979  11.00000  0.05    0.95
Q13   1   0.4421  0.5565  0.2167  11.00000  0.05    0.86
Q14   1   0.3419  0.6521  0.7974  11.00000  0.05    0.86
Q15   1   0.2408  0.7354  0.6540  11.00000  0.05    0.86
Q16   1   0.6503  0.5279  0.4810  11.00000  0.05    0.82
Q17   1   0.2604  0.5093  0.1823  11.00000  0.05    0.81
Q18   1   0.6315  0.5851  0.3411  11.00000  0.05    0.80
Q19   1   0.7484  0.6215  0.3111  11.00000  0.05    0.78
Q20   1   0.1881  0.7399  0.9376  11.00000  0.05    0.77

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0417 for 7053 Fo > 4sig(Fo) and 0.0486 for all 25251 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 3.85, deepest hole -1.38
  REM Mean Shift 0, Max Shift -0.002.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0486
  REM R1_gt = 0.0417
  REM wR_ref = 0.1117
  REM GOOF = 1.029
  REM Shift_max = -0.002
  REM Shift_mean = 0
  REM Reflections_all = 25251
  REM Reflections_gt = 7053
  REM Parameters = n/a
  REM Hole = -1.38
  REM Peak = 3.85
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.134
_oxdiff_exptl_absorpt_empirical_full_min 0.571
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
####################################################################### 
# 
# 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_moocl3(phs(ch2)2sph)
_database_code_depnum_ccdc_archive 'CCDC 2050669'
loop_
_audit_author_name
_audit_author_address
'Danielle Smith'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2020-12-16 deposited with the CCDC.	2021-02-26 downloaded from the CCDC.
;
_audit_creation_date             2020-06-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        '[MoOCl3(PhS(CH2)2SPh)]'
_chemical_formula_moiety         'C14 H14 Cl3 Mo O S2'
_chemical_formula_sum            'C14 H14 Cl3 Mo O S2'
_chemical_formula_weight         464.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         MoOCl3S2C14H14
_chemical_oxdiff_usercomment     'Orange Block'
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'
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'
O O 0.0106 0.0060 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   19.6139(2)
_cell_length_b                   6.80640(10)
_cell_length_c                   12.9677(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.1600(10)
_cell_angle_gamma                90
_cell_volume                     1721.19(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    43730
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.9380
_cell_measurement_theta_min      2.1980
_shelx_estimated_absorpt_T_max   0.758
_shelx_estimated_absorpt_T_min   0.668
_exptl_absorpt_coefficient_mu    1.464
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             924
_exptl_crystal_preparation       'Slow evporation from DCM'
_exptl_crystal_recrystallization_method 'Slow evporation from DCM'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            64024
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.878
_diffrn_reflns_theta_min         3.134
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -98.00  21.00   0.50    0.50    --   -8.30 -57.00 -30.00  238
  2  ω    -98.00  22.00   0.50    0.50    --   -8.30 -60.00  90.00  240
  3  ω    -98.00  81.00   0.50    0.50    --   -8.30   0.00-150.00  358
  4  ω    -98.00  21.00   0.50    0.50    --   -8.30 -57.00-120.00  238
  5  ω    -39.00  81.00   0.50    0.50    --   -8.30  60.00 -90.00  240
  6  ω    -39.00  81.00   0.50    0.50    --   -8.30  60.00  60.00  240
  7  ω    -39.00  81.00   0.50    0.50    --   -8.30  60.00-180.00  240
  8  ω    -39.00  81.00   0.50    0.50    --   -8.30  60.00 -30.00  240
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0210969000
_diffrn_orient_matrix_UB_12      0.0289177000
_diffrn_orient_matrix_UB_13      -0.0453316000
_diffrn_orient_matrix_UB_21      0.0286173000
_diffrn_orient_matrix_UB_22      -0.0055341000
_diffrn_orient_matrix_UB_23      -0.0290226000
_diffrn_orient_matrix_UB_31      -0.0076776000
_diffrn_orient_matrix_UB_32      -0.0999298000
_diffrn_orient_matrix_UB_33      -0.0114469000
_diffrn_oxdiff_digest_frames     
;
01614156ee8d529e13a1e93bdff17fdd73000564394
;
_diffrn_oxdiff_digest_hkl        
;
01858ed693473f774e39cf6b517cd863a236f1
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5485
_reflns_number_total             5833
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.437
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         5833
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0542
_refine_ls_restrained_S_all      1.472
_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)+7.6691P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1250
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Mo1-Cl2 \\sim Mo-Cl2
 with sigma of 0.02
 Mo1-S1 \\sim Mo-S1
 with sigma of 0.02
 Mo1-O1 \\sim Mo-O1
 with sigma of 0.02
 Mo1-Cl3 \\sim Mo-Cl3
 with sigma of 0.02
3. Others
 Fixed Sof: Mo1(0.47051) O1(0.47051) Cl3(0.47051) Mo(0.52949) O1A(0.52949)
 Cl1A(0.52949)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C5(H5), C3(H3), C14(H14), C10(H10), C4(H4), C11(H11),
 C12(H12), C13(H13)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.73985(4) 0.39207(12) 0.77994(6) 0.01413(14) Uani 0.4705 1 d D . P A 1
Cl2 Cl 0.65815(4) 0.23846(13) 0.65499(7) 0.01912(16) Uani 1 1 d D . . . .
S2 S 0.79764(4) 0.41640(14) 0.58270(7) 0.01833(17) Uani 1 1 d . . . . .
S1 S 0.69498(5) 0.72193(13) 0.71288(7) 0.01772(16) Uani 1 1 d D . . . .
O1 O 0.6934(7) 0.4121(18) 0.8834(11) 0.021(2) Uani 0.4705 1 d D . P A 1
Cl3 Cl 0.80210(12) 0.1041(3) 0.80276(19) 0.0185(4) Uani 0.4705 1 d D . P A 1
C1 C 0.60782(18) 0.7035(6) 0.6581(3) 0.0207(7) Uani 1 1 d . . . . .
C7 C 0.74179(19) 0.7880(5) 0.6058(3) 0.0191(6) Uani 1 1 d . . . . .
H7A H 0.719240 0.899050 0.569838 0.023 Uiso 1 1 calc R . . . .
H7B H 0.787531 0.829586 0.632958 0.023 Uiso 1 1 calc R . . . .
C9 C 0.88408(19) 0.5032(7) 0.5999(3) 0.0235(8) Uani 1 1 d . . . . .
C8 C 0.74778(19) 0.6228(6) 0.5283(3) 0.0193(7) Uani 1 1 d . . . . .
H8A H 0.768918 0.673708 0.469523 0.023 Uiso 1 1 calc R . . . .
H8B H 0.702146 0.577380 0.503023 0.023 Uiso 1 1 calc R . . . .
C2 C 0.5626(2) 0.6277(6) 0.7238(4) 0.0277(8) Uani 1 1 d . . . . .
H2 H 0.578760 0.582666 0.789569 0.033 Uiso 1 1 calc R . . . .
C6 C 0.5843(2) 0.7693(6) 0.5592(3) 0.0270(8) Uani 1 1 d . . . . .
H6 H 0.614679 0.819518 0.515618 0.032 Uiso 1 1 calc R . . . .
C5 C 0.5147(2) 0.7587(7) 0.5267(4) 0.0351(10) Uani 1 1 d . . . . .
H5 H 0.498398 0.801723 0.460533 0.042 Uiso 1 1 calc R . . . .
C3 C 0.4929(2) 0.6202(7) 0.6897(4) 0.0362(11) Uani 1 1 d . . . . .
H3 H 0.462122 0.571297 0.733175 0.043 Uiso 1 1 calc R . . . .
C14 C 0.9322(2) 0.3686(8) 0.6424(3) 0.0323(10) Uani 1 1 d . . . . .
H14 H 0.918376 0.244665 0.662109 0.039 Uiso 1 1 calc R . . . .
C10 C 0.9044(2) 0.6881(8) 0.5703(3) 0.0316(9) Uani 1 1 d . . . . .
H10 H 0.872090 0.777783 0.541267 0.038 Uiso 1 1 calc R . . . .
C4 C 0.4692(2) 0.6854(7) 0.5911(5) 0.0382(11) Uani 1 1 d . . . . .
H4 H 0.422669 0.679771 0.568406 0.046 Uiso 1 1 calc R . . . .
C11 C 0.9735(3) 0.7382(10) 0.5846(4) 0.0464(15) Uani 1 1 d . . . . .
H11 H 0.987427 0.862322 0.565381 0.056 Uiso 1 1 calc R . . . .
C12 C 1.0212(2) 0.6050(11) 0.6269(4) 0.0502(17) Uani 1 1 d . . . . .
H12 H 1.067345 0.639736 0.636395 0.060 Uiso 1 1 calc R . . . .
C13 C 1.0012(2) 0.4199(11) 0.6555(4) 0.0465(15) Uani 1 1 d . . . . .
H13 H 1.033753 0.329858 0.683320 0.056 Uiso 1 1 calc R . . . .
Mo Mo 0.75628(3) 0.34439(10) 0.75352(5) 0.01189(12) Uani 0.5295 1 d D . P A 2
O1A O 0.8017(3) 0.1380(10) 0.7626(5) 0.0206(12) Uani 0.5295 1 d . . P A 2
Cl1A Cl 0.6966(2) 0.3567(6) 0.8988(4) 0.0208(6) Uani 0.5295 1 d . . P A 2
Cl1 Cl 0.83786(4) 0.57169(14) 0.83483(7) 0.02043(17) Uani 1 1 d . . . . .

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 0.0125(3) 0.0154(3) 0.0147(3) 0.0016(2) 0.0025(2) -0.0015(2)
Cl2 0.0127(3) 0.0154(4) 0.0287(4) -0.0008(3) 0.0001(3) 0.0002(3)
S2 0.0158(4) 0.0183(4) 0.0211(4) -0.0009(3) 0.0031(3) 0.0021(3)
S1 0.0186(4) 0.0151(4) 0.0196(4) 0.0004(3) 0.0029(3) 0.0013(3)
O1 0.013(3) 0.030(7) 0.020(6) -0.004(4) 0.004(3) 0.002(5)
Cl3 0.0171(8) 0.0147(10) 0.0230(11) 0.0033(8) -0.0008(8) -0.0005(7)
C1 0.0160(15) 0.0175(16) 0.0284(18) -0.0012(14) 0.0018(13) 0.0052(12)
C7 0.0219(16) 0.0148(16) 0.0213(16) 0.0015(12) 0.0049(12) -0.0007(13)
C9 0.0146(15) 0.038(2) 0.0192(16) -0.0007(15) 0.0065(12) -0.0023(14)
C8 0.0200(16) 0.0191(16) 0.0187(15) 0.0017(13) 0.0009(12) 0.0019(13)
C2 0.0174(17) 0.027(2) 0.040(2) 0.0002(17) 0.0082(15) 0.0057(15)
C6 0.0277(19) 0.0168(17) 0.035(2) 0.0012(15) -0.0045(16) 0.0035(15)
C5 0.031(2) 0.024(2) 0.048(3) 0.0002(19) -0.0115(19) 0.0056(17)
C3 0.0186(18) 0.029(2) 0.062(3) -0.006(2) 0.0093(19) 0.0052(16)
C14 0.0206(18) 0.055(3) 0.0224(18) 0.0033(19) 0.0083(14) 0.0091(18)
C10 0.031(2) 0.042(3) 0.0225(18) -0.0013(17) 0.0072(15) -0.0130(19)
C4 0.0227(19) 0.024(2) 0.065(3) -0.008(2) -0.006(2) 0.0060(16)
C11 0.038(3) 0.074(4) 0.030(2) -0.011(2) 0.0149(19) -0.031(3)
C12 0.0196(19) 0.107(5) 0.025(2) -0.016(3) 0.0093(16) -0.017(3)
C13 0.0174(18) 0.100(5) 0.0222(19) -0.005(3) 0.0042(15) 0.011(2)
Mo 0.0086(3) 0.0134(3) 0.0140(3) 0.0014(2) 0.00295(19) 0.0008(2)
O1A 0.015(2) 0.018(3) 0.029(3) 0.007(3) 0.003(3) 0.003(2)
Cl1A 0.0176(10) 0.0296(18) 0.0160(11) 0.0064(11) 0.0058(7) 0.0018(12)
Cl1 0.0158(3) 0.0252(4) 0.0205(4) -0.0032(3) 0.0029(3) -0.0044(3)

_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 2.3936(11) . ?
Mo1 S1 2.5313(12) . ?
Mo1 O1 1.706(15) . ?
Mo1 Cl3 2.311(3) . ?
Mo1 Cl1 2.3244(11) . ?
Cl2 Mo 2.3086(10) . ?
S2 C9 1.787(4) . ?
S2 C8 1.811(4) . ?
S2 Mo 2.4881(11) . ?
S1 C1 1.784(4) . ?
S1 C7 1.802(4) . ?
S1 Mo 2.8619(11) . ?
C1 C2 1.393(6) . ?
C1 C6 1.390(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.521(5) . ?
C9 C14 1.386(6) . ?
C9 C10 1.387(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C2 H2 0.9300 . ?
C2 C3 1.392(6) . ?
C6 H6 0.9300 . ?
C6 C5 1.387(6) . ?
C5 H5 0.9300 . ?
C5 C4 1.379(8) . ?
C3 H3 0.9300 . ?
C3 C4 1.385(8) . ?
C14 H14 0.9300 . ?
C14 C13 1.390(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.390(6) . ?
C4 H4 0.9300 . ?
C11 H11 0.9300 . ?
C11 C12 1.375(9) . ?
C12 H12 0.9300 . ?
C12 C13 1.383(10) . ?
C13 H13 0.9300 . ?
Mo O1A 1.661(7) . ?
Mo Cl1A 2.323(5) . ?
Mo Cl1 2.3881(11) . ?

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 S1 88.39(4) . . ?
O1 Mo1 Cl2 101.1(5) . . ?
O1 Mo1 S1 90.2(3) . . ?
O1 Mo1 Cl3 106.6(3) . . ?
O1 Mo1 Cl1 102.2(5) . . ?
Cl3 Mo1 Cl2 91.28(7) . . ?
Cl3 Mo1 S1 162.85(8) . . ?
Cl3 Mo1 Cl1 89.93(7) . . ?
Cl1 Mo1 Cl2 155.32(5) . . ?
Cl1 Mo1 S1 83.36(4) . . ?
C9 S2 C8 104.94(19) . . ?
C9 S2 Mo 110.47(13) . . ?
C8 S2 Mo 106.59(13) . . ?
C1 S1 Mo1 110.94(13) . . ?
C1 S1 C7 104.88(18) . . ?
C1 S1 Mo 112.08(13) . . ?
C7 S1 Mo1 107.39(12) . . ?
C7 S1 Mo 97.30(12) . . ?
C2 C1 S1 115.4(3) . . ?
C6 C1 S1 123.6(3) . . ?
C6 C1 C2 120.8(4) . . ?
S1 C7 H7A 108.8 . . ?
S1 C7 H7B 108.8 . . ?
H7A C7 H7B 107.6 . . ?
C8 C7 S1 114.0(3) . . ?
C8 C7 H7A 108.8 . . ?
C8 C7 H7B 108.8 . . ?
C14 C9 S2 115.3(4) . . ?
C14 C9 C10 120.4(4) . . ?
C10 C9 S2 124.2(3) . . ?
S2 C8 H8A 109.0 . . ?
S2 C8 H8B 109.0 . . ?
C7 C8 S2 113.1(2) . . ?
C7 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C1 C2 H2 120.4 . . ?
C1 C2 C3 119.2(4) . . ?
C3 C2 H2 120.4 . . ?
C1 C6 H6 120.6 . . ?
C5 C6 C1 118.9(4) . . ?
C5 C6 H6 120.6 . . ?
C6 C5 H5 119.6 . . ?
C4 C5 C6 120.9(5) . . ?
C4 C5 H5 119.6 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.1(5) . . ?
C4 C3 H3 120.0 . . ?
C9 C14 H14 120.2 . . ?
C9 C14 C13 119.6(5) . . ?
C13 C14 H14 120.2 . . ?
C9 C10 H10 120.3 . . ?
C9 C10 C11 119.4(5) . . ?
C11 C10 H10 120.3 . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C10 C11 H11 119.9 . . ?
C12 C11 C10 120.3(6) . . ?
C12 C11 H11 119.9 . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.4(4) . . ?
C13 C12 H12 119.8 . . ?
C14 C13 H13 120.1 . . ?
C12 C13 C14 119.8(5) . . ?
C12 C13 H13 120.1 . . ?
Cl2 Mo S2 84.31(4) . . ?
Cl2 Mo S1 82.51(3) . . ?
Cl2 Mo Cl1A 89.84(13) . . ?
Cl2 Mo Cl1 157.82(4) . . ?
S2 Mo S1 80.20(3) . . ?
O1A Mo Cl2 100.6(2) . . ?
O1A Mo S2 90.4(2) . . ?
O1A Mo S1 169.8(2) . . ?
O1A Mo Cl1A 106.6(2) . . ?
O1A Mo Cl1 100.8(2) . . ?
Cl1A Mo S2 162.83(9) . . ?
Cl1A Mo S1 83.03(9) . . ?
Cl1A Mo Cl1 89.47(13) . . ?
Cl1 Mo S2 89.91(4) . . ?
Cl1 Mo S1 75.40(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 S1 C1 C2 56.1(3) . . . . ?
Mo1 S1 C1 C6 -127.5(3) . . . . ?
Mo1 S1 C7 C8 46.6(3) . . . . ?
S2 C9 C14 C13 177.8(3) . . . . ?
S2 C9 C10 C11 -178.1(3) . . . . ?
S1 C1 C2 C3 175.8(3) . . . . ?
S1 C1 C6 C5 -176.1(3) . . . . ?
S1 C7 C8 S2 -65.0(3) . . . . ?
C1 S1 C7 C8 -71.5(3) . . . . ?
C1 C2 C3 C4 0.8(7) . . . . ?
C1 C6 C5 C4 0.3(7) . . . . ?
C7 S1 C1 C2 171.7(3) . . . . ?
C7 S1 C1 C6 -11.9(4) . . . . ?
C9 S2 C8 C7 -71.1(3) . . . . ?
C9 C14 C13 C12 0.6(7) . . . . ?
C9 C10 C11 C12 0.4(7) . . . . ?
C8 S2 C9 C14 179.3(3) . . . . ?
C8 S2 C9 C10 -3.1(4) . . . . ?
C2 C1 C6 C5 0.1(6) . . . . ?
C2 C3 C4 C5 -0.3(7) . . . . ?
C6 C1 C2 C3 -0.7(6) . . . . ?
C6 C5 C4 C3 -0.3(7) . . . . ?
C14 C9 C10 C11 -0.6(6) . . . . ?
C10 C9 C14 C13 0.0(6) . . . . ?
C10 C11 C12 C13 0.2(7) . . . . ?
C11 C12 C13 C14 -0.7(7) . . . . ?
Mo S2 C9 C14 64.8(3) . . . . ?
Mo S2 C9 C10 -117.6(3) . . . . ?
Mo S2 C8 C7 46.2(3) . . . . ?
Mo S1 C1 C2 67.2(3) . . . . ?
Mo S1 C1 C6 -116.3(3) . . . . ?
Mo S1 C7 C8 43.8(3) . . . . ?

_iucr_refine_instructions_details 
;
TITL moocl3(phs(ch2)2sph)_a.res in P2(1)/c
    moocl3(phs(ch2)2sph).res
    created by SHELXL-2018/3 at 11:16:22 on 12-Jun-2020
REM Old TITL moocl3(phs(ch2)2sph)_a.res in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.316, Rweak 0.067, Alpha 0.105
REM <I/s> 3.990 for 313 systematic absences, Orientation as input
REM Formula found by SHELXT: C14 S2 Cl3 Mo O1 H14
CELL 0.71073 19.6139 6.8064 12.9677 90 96.16 90
ZERR 4 0.0002 0.0001 0.0002 0 0.001 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl Mo O S
UNIT 56 56 12 4 4 8
SADI Mo1 Cl2 Mo Cl2
SADI Mo1 S1 Mo S1
SADI Mo1 O1 Mo O1
SADI Mo1 Cl3 Mo Cl3

L.S. 10
PLAN  5
SIZE 0.3 0.3 0.2
CONF
list 4
MORE -1
BOND $H
fmap 2
acta
OMIT 2 0 0
OMIT -15 0 2
OMIT -19 0 6
OMIT -17 0 6
REM <olex2.extras>
REM <HklSrc "%.\\MoOCl3(PhS(CH2)2SPh).hkl">
REM </olex2.extras>

WGHT    0.000000    7.669100
FVAR       0.35392
PART 1
MO1   4    0.739853    0.392068    0.779944    10.47051    0.01248    0.01543 =
         0.01470    0.00156    0.00252   -0.00152
PART 0
CL2   3    0.658149    0.238465    0.654990    11.00000    0.01270    0.01544 =
         0.02874   -0.00079    0.00007    0.00019
S2    6    0.797642    0.416404    0.582698    11.00000    0.01583    0.01826 =
         0.02114   -0.00092    0.00313    0.00214
S1    6    0.694981    0.721926    0.712880    11.00000    0.01864    0.01513 =
         0.01957    0.00037    0.00292    0.00131
PART 1
O1    5    0.693417    0.412145    0.883423    10.47051    0.01340    0.03025 =
         0.01983   -0.00405    0.00360    0.00215
CL3   3    0.802102    0.104085    0.802764    10.47051    0.01707    0.01467 =
         0.02301    0.00332   -0.00080   -0.00045
PART 0
C1    1    0.607821    0.703501    0.658140    11.00000    0.01600    0.01753 =
         0.02842   -0.00118    0.00177    0.00521
C7    1    0.741795    0.787975    0.605839    11.00000    0.02185    0.01483 =
         0.02127    0.00148    0.00487   -0.00072
AFIX  23
H7A   2    0.719240    0.899050    0.569838    11.00000   -1.20000
H7B   2    0.787531    0.829586    0.632958    11.00000   -1.20000
AFIX   0
C9    1    0.884084    0.503161    0.599878    11.00000    0.01460    0.03757 =
         0.01923   -0.00073    0.00655   -0.00228
C8    1    0.747777    0.622759    0.528297    11.00000    0.01995    0.01909 =
         0.01872    0.00168    0.00092    0.00193
AFIX  23
H8A   2    0.768918    0.673708    0.469523    11.00000   -1.20000
H8B   2    0.702146    0.577380    0.503023    11.00000   -1.20000
AFIX   0
C2    1    0.562581    0.627719    0.723759    11.00000    0.01742    0.02709 =
         0.03974    0.00020    0.00819    0.00571
AFIX  43
H2    2    0.578760    0.582666    0.789569    11.00000   -1.20000
AFIX   0
C6    1    0.584276    0.769287    0.559242    11.00000    0.02771    0.01680 =
         0.03472    0.00116   -0.00448    0.00354
AFIX  43
H6    2    0.614679    0.819518    0.515618    11.00000   -1.20000
AFIX   0
C5    1    0.514655    0.758749    0.526707    11.00000    0.03061    0.02377 =
         0.04755    0.00022   -0.01152    0.00563
AFIX  43
H5    2    0.498398    0.801723    0.460533    11.00000   -1.20000
AFIX   0
C3    1    0.492861    0.620183    0.689707    11.00000    0.01858    0.02932 =
         0.06167   -0.00637    0.00927    0.00522
AFIX  43
H3    2    0.462122    0.571297    0.733175    11.00000   -1.20000
AFIX   0
C14   1    0.932184    0.368588    0.642409    11.00000    0.02062    0.05535 =
         0.02235    0.00333    0.00832    0.00914
AFIX  43
H14   2    0.918376    0.244665    0.662109    11.00000   -1.20000
AFIX   0
C10   1    0.904390    0.688091    0.570338    11.00000    0.03095    0.04215 =
         0.02252   -0.00131    0.00719   -0.01300
AFIX  43
H10   2    0.872090    0.777783    0.541267    11.00000   -1.20000
AFIX   0
C4    1    0.469237    0.685429    0.591148    11.00000    0.02270    0.02423 =
         0.06516   -0.00793   -0.00616    0.00600
AFIX  43
H4    2    0.422669    0.679771    0.568406    11.00000   -1.20000
AFIX   0
C11   1    0.973470    0.738226    0.584569    11.00000    0.03791    0.07383 =
         0.02997   -0.01098    0.01486   -0.03139
AFIX  43
H11   2    0.987427    0.862322    0.565381    11.00000   -1.20000
AFIX   0
C12   1    1.021237    0.605043    0.626903    11.00000    0.01959    0.10723 =
         0.02516   -0.01628    0.00930   -0.01744
AFIX  43
H12   2    1.067345    0.639736    0.636395    11.00000   -1.20000
AFIX   0
C13   1    1.001171    0.419883    0.655453    11.00000    0.01745    0.10042 =
         0.02223   -0.00497    0.00419    0.01133
AFIX  43
H13   2    1.033753    0.329858    0.683320    11.00000   -1.20000
AFIX   0
PART 2
MO    4    0.756285    0.344393    0.753519    10.52949    0.00863    0.01342 =
         0.01400    0.00137    0.00295    0.00084
O1A   5    0.801715    0.138022    0.762621    10.52949    0.01468    0.01827 =
         0.02892    0.00655    0.00299    0.00252
CL1A  3    0.696617    0.356678    0.898751    10.52949    0.01756    0.02960 =
         0.01601    0.00637    0.00584    0.00179
PART 0
CL1   3    0.837860    0.571686    0.834830    11.00000    0.01584    0.02521 =
         0.02045   -0.00316    0.00289   -0.00437
HKLF 4




REM  moocl3(phs(ch2)2sph)_a.res in P2(1)/c
REM wR2 = 0.1250, GooF = S = 1.437, Restrained GooF = 1.472 for all data
REM R1 = 0.0542 for 5485 Fo > 4sig(Fo) and 0.0580 for all 5833 data
REM 217 parameters refined using 2 restraints

END  
     
WGHT      0.0000      7.6536 

REM Highest difference peak  0.735,  deepest hole -0.869,  1-sigma level  0.121
Q1    1   0.7345  0.8091  0.7791  11.00000  0.05    0.73
Q2    1   0.7367  0.3616  0.8436  11.00000  0.05    0.67
Q3    1   0.8622  0.1089  0.6158  11.00000  0.05    0.62
Q4    1   0.7809  0.3889  0.6749  11.00000  0.05    0.58
Q5    1   0.7284  0.3895  0.6605  11.00000  0.05    0.53

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0542 for 5485 Fo > 4sig(Fo) and 0.0580 for all 67243 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.73, deepest hole -0.87
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0580
  REM R1_gt = 0.0542
  REM wR_ref = 0.1250
  REM GOOF = 1.437
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 67243
  REM Reflections_gt = 5485
  REM Parameters = n/a
  REM Hole = -0.87
  REM Peak = 0.73
  REM Flack = n/a

  
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.686
_oxdiff_exptl_absorpt_empirical_full_min 0.620
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
