# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_sattelberger_04
_database_code_depnum_ccdc_archive 'CCDC 2151144'
loop_
_audit_author_name
_audit_author_address
'Thomas Shaw'
;University of Central Florida
United States of America
;
_audit_update_record             
;
2022-02-09 deposited with the CCDC.	2022-04-22 downloaded from the CCDC.
;
_audit_creation_date             2022-02-08
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        Tetrachloro(1,2-dimethoxyethane)tungsten(IV)
_chemical_formula_moiety         'C4 H10 Cl4 O2 W'
_chemical_formula_sum            'C4 H10 Cl4 O2 W'
_chemical_formula_weight         415.77
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         WCl4CNO
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   8.0766(2)
_cell_length_b                   11.3089(2)
_cell_length_c                   11.7413(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.687(2)
_cell_angle_gamma                90
_cell_volume                     1072.34(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16956
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      33.8020
_cell_measurement_theta_min      3.0780
_shelx_estimated_absorpt_T_max   0.799
_shelx_estimated_absorpt_T_min   0.555
_exptl_absorpt_coefficient_mu    11.724
_exptl_absorpt_correction_T_max  0.705
_exptl_absorpt_correction_T_min  0.450
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.90a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.575
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             768
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 1 0.0172
1 0 -1 0.0172
0 1 0 0.0148
0 -1 0 0.0188
-1 1 -1 0.0102
1 -1 1 0.0102
1 -1 -1 0.0122

_exptl_crystal_recrystallization_method 
'Single crystals were obtained by allowing tungsten(IV) chloride to sit in excess 1,2-dimethoxyethane overnight'
_exptl_crystal_size_max          0.057
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.02
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0000 0.0008 1.0014 -0.0125 0.0018 0.1053
1.0000 -0.0008 -1.0014 0.0125 -0.0018 -0.1053
-0.0002 0.9995 -0.0012 -0.0365 -0.0509 -0.0035
0.0002 -0.9995 0.0012 0.0365 0.0509 0.0035
-0.9998 0.9990 -1.0011 0.0396 -0.1087 0.0451
0.9998 -0.9990 1.0011 -0.0396 0.1087 -0.0451
1.0002 -1.0003 -1.0002 0.0490 0.0491 -0.1018

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19395
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.900
_diffrn_reflns_theta_min         3.100
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -2.00  42.00   0.50   19.82    --   13.12  85.00  25.00   88
  2  ω     14.00  40.00   0.50   19.82    --   13.12 -85.00 -93.00   52
  3  ω    -41.00  -2.00   0.50   19.82    --  -13.59 -85.00 -93.00   78
  4  ω    -40.00   6.00   0.50   19.82    --  -13.59  85.00  25.00   92
  5  ω      2.00  80.00   0.50   19.82    --   13.12  37.00-180.00  156
  6  ω    -23.00   3.00   0.50   19.82    --   13.12 -99.00-120.00   52
  7  ω    -58.00   5.00   0.50   19.82    --   13.12 -19.00   0.00  126
  8  ω    -60.00   4.00   0.50   19.82    --   13.12 -19.00  60.00  128
  9  ω    -22.00  47.00   0.50   19.82    --   13.12 -99.00 150.00  138
 10  ω     22.00  47.00   0.50   19.82    --   13.12 -99.00-120.00   50
 11  ω     -2.00  75.00   0.50   19.82    --   13.12  57.00-150.00  154
 12  ω    -42.00   3.00   0.50   19.82    --   13.12 -19.00-180.00   90
 13  ω    -20.00   6.00   0.50   19.82    --   13.12 -99.00  60.00   52
 14  ω     18.00  47.00   0.50   19.82    --   13.12 -99.00  60.00   58
 15  ω     28.00  54.00   0.50   19.82    --   13.12-112.00-138.69   52
 16  ω    -77.00 -37.00   0.50   19.82    --  -13.59 -37.00-150.00   80
 17  ω    -82.00   1.00   0.50   19.82    --  -13.59 -57.00 -60.00  166
 18  ω    -26.00  60.00   0.50   19.82    --  -13.59  37.00 -60.00  172
 19  ω    -54.00 -29.00   0.50   19.82    --  -13.59 111.00 -87.30   50
 20  ω    -34.00  -3.00   0.50   19.82    --  -13.59 -37.00-150.00   62
 21  ω    -85.00 -15.00   0.50   19.82    --  -13.59 -19.00   0.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0318238000
_diffrn_orient_matrix_UB_12      -0.0365667000
_diffrn_orient_matrix_UB_13      -0.0442225000
_diffrn_orient_matrix_UB_21      0.0280442000
_diffrn_orient_matrix_UB_22      -0.0508424000
_diffrn_orient_matrix_UB_23      0.0298182000
_diffrn_orient_matrix_UB_31      -0.0769449000
_diffrn_orient_matrix_UB_32      -0.0034466000
_diffrn_orient_matrix_UB_33      0.0283245000
_diffrn_oxdiff_digest_frames     
;
01697f635f62e1e179d1b1a2f7f0edc182020362e7b
;
_diffrn_oxdiff_digest_hkl        
;
01fa466dd2f53ebea48edc0a2f69b8737ac4ea
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.894
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.830
_reflns_number_gt                3678
_reflns_number_total             3809
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.322
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.178
_refine_ls_abs_structure_details 
;
 Flack x determined using 1709 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         3809
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0224
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0350P)²+1.1463P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0558
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H4A(0.054) H4B(0.054) H4C(0.054) H3A(0.031) H3B(0.031) H2A(0.028)
 H2B(0.028) H1A(0.038) H1B(0.038) H1C(0.038)
 Fixed X: H4A(0.318963) H4B(0.512101) H4C(0.387337) H3A(0.517688)
 H3B(0.614457) H2A(0.475734) H2B(0.549374) H1A(0.155169) H1B(0.34839)
 H1C(0.258894)
 Fixed Y: H4A(0.524906) H4B(0.556342) H4C(0.637453) H3A(0.800308)
 H3B(0.705772) H2A(0.76945) H2B(0.885346) H1A(0.986968) H1B(1.012415)
 H1C(0.911084)
 Fixed Z: H4A(0.341685) H4B(0.346829) H4C(0.274318) H3A(0.393248)
 H3B(0.471546) H2A(0.632945) H2B(0.572519) H1A(0.618328) H1B(0.637629)
 H1C(0.709435)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
W1 W 0.13325(5) 0.73637(2) 0.48051(4) 0.01576(6) Uani 1 1 d . . . . .
Cl1 Cl 0.16206(18) 0.83271(13) 0.30557(12) 0.0208(3) Uani 1 1 d . . . . .
Cl2 Cl -0.09985(19) 0.84439(18) 0.52853(15) 0.0292(3) Uani 1 1 d . . . . .
Cl3 Cl -0.0172(2) 0.58111(17) 0.40231(15) 0.0349(4) Uani 1 1 d . . . . .
Cl4 Cl 0.15694(19) 0.64550(14) 0.65882(12) 0.0234(3) Uani 1 1 d . . . . .
O1 O 0.3021(5) 0.8653(4) 0.5477(4) 0.0181(8) Uani 1 1 d . . . . .
O2 O 0.3726(6) 0.6631(4) 0.4434(4) 0.0224(9) Uani 1 1 d . . . . .
C4 C 0.4000(11) 0.5894(7) 0.3433(6) 0.0360(17) Uani 1 1 d . . . . .
H4A H 0.318963 0.524906 0.341685 0.054 Uiso 1 1 calc GR . . . .
H4B H 0.512101 0.556342 0.346829 0.054 Uiso 1 1 calc GR . . . .
H4C H 0.387337 0.637453 0.274318 0.054 Uiso 1 1 calc GR . . . .
C3 C 0.5082(10) 0.7481(6) 0.4606(8) 0.0258(14) Uani 1 1 d . . . . .
H3A H 0.517688 0.800308 0.393248 0.031 Uiso 1 1 calc R . . . .
H3B H 0.614457 0.705772 0.471546 0.031 Uiso 1 1 calc R . . . .
C2 C 0.4695(7) 0.8195(6) 0.5638(6) 0.0232(12) Uani 1 1 d . . . . .
H2A H 0.475734 0.769450 0.632945 0.028 Uiso 1 1 calc R . . . .
H2B H 0.549374 0.885346 0.572519 0.028 Uiso 1 1 calc R . . . .
C1 C 0.2630(8) 0.9509(6) 0.6354(6) 0.0255(12) Uani 1 1 d . . . . .
H1A H 0.155169 0.986968 0.618328 0.038 Uiso 1 1 calc GR . . . .
H1B H 0.348390 1.012415 0.637629 0.038 Uiso 1 1 calc GR . . . .
H1C H 0.258894 0.911084 0.709435 0.038 Uiso 1 1 calc GR . . . .


_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
W1 Cl1 2.3391(15) . ?
W1 Cl2 2.3195(17) . ?
W1 Cl3 2.3185(16) . ?
W1 Cl4 2.3380(15) . ?
W1 O1 2.141(4) . ?
W1 O2 2.152(5) . ?
O1 C2 1.458(7) . ?
O1 C1 1.451(7) . ?
O2 C4 1.460(8) . ?
O2 C3 1.469(9) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C2 1.493(10) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 W1 Cl1 93.31(6) . . ?
Cl2 W1 Cl4 94.11(6) . . ?
Cl3 W1 Cl1 93.57(6) . . ?
Cl3 W1 Cl2 94.13(8) . . ?
Cl3 W1 Cl4 93.36(6) . . ?
Cl4 W1 Cl1 169.45(6) . . ?
O1 W1 Cl1 86.36(12) . . ?
O1 W1 Cl2 93.85(12) . . ?
O1 W1 Cl3 172.01(13) . . ?
O1 W1 Cl4 85.68(12) . . ?
O1 W1 O2 76.52(17) . . ?
O2 W1 Cl1 84.40(13) . . ?
O2 W1 Cl2 170.20(13) . . ?
O2 W1 Cl3 95.51(14) . . ?
O2 W1 Cl4 87.03(13) . . ?
C2 O1 W1 113.0(4) . . ?
C1 O1 W1 124.9(4) . . ?
C1 O1 C2 110.8(5) . . ?
C4 O2 W1 121.9(5) . . ?
C4 O2 C3 111.3(6) . . ?
C3 O2 W1 113.0(4) . . ?
O2 C4 H4A 109.5 . . ?
O2 C4 H4B 109.5 . . ?
O2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O2 C3 H3A 110.2 . . ?
O2 C3 H3B 110.2 . . ?
O2 C3 C2 107.6(6) . . ?
H3A C3 H3B 108.5 . . ?
C2 C3 H3A 110.2 . . ?
C2 C3 H3B 110.2 . . ?
O1 C2 C3 106.8(5) . . ?
O1 C2 H2A 110.4 . . ?
O1 C2 H2B 110.4 . . ?
C3 C2 H2A 110.4 . . ?
C3 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
H1A 14 H1B 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
W1 O1 C2 C3 43.2(6) . . . . ?
W1 O2 C3 C2 38.4(7) . . . . ?
O2 C3 C2 O1 -52.1(7) . . . . ?
C4 O2 C3 C2 179.8(6) . . . . ?
C1 O1 C2 C3 -171.0(5) . . . . ?


_olex2_date_sample_data_collection 2021-04-16
_olex2_date_sample_submission    2021-04-14
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder with Paratone oil'
_olex2_submission_original_sample_id Sattelberger_04
_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 1.343
_oxdiff_exptl_absorpt_empirical_full_min 0.805
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_235
_database_code_depnum_ccdc_archive 'CCDC 2151146'
loop_
_audit_author_name
_audit_author_address
'Thomas Shaw'
;University of Central Florida
United States of America
;
_audit_update_record             
;
2022-02-09 deposited with the CCDC.	2022-04-22 downloaded from the CCDC.
;
_audit_creation_date             2021-08-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'Tetrachlorobis(diethyl ether)molybdenum(IV)'
_chemical_formula_moiety         'C8 H20 Cl4 Mo O2'
_chemical_formula_sum            'C8 H20 Cl4 Mo O2'
_chemical_formula_weight         385.98
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Mo C Cl O'
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'

_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                   7.5956(2)
_cell_length_b                   11.4732(4)
_cell_length_c                   9.0193(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.347(3)
_cell_angle_gamma                90
_cell_volume                     754.22(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4082
_cell_measurement_temperature    298.1(5)
_cell_measurement_theta_max      30.3800
_cell_measurement_theta_min      2.9410
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.560
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             388
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 -10 10 0.1215
0 10 10 0.0642
2 10 -10 0.1370
0 -11 -9 0.0722
-11 -3 3 0.1209
3 10 -10 0.1314
10 5 -5 0.1936
0 -10 10 0.1260
8 8 -8 0.1723
-6 -10 -5 0.0841
-9 -7 -1 0.0973
7 0 7 0.2078
7 11 -5 0.1741
6 -5 -11 0.0947
3 -15 3 0.1503
-5 0 12 0.1324
-8 5 10 0.1296
9 -7 1 0.2284
7 11 0 0.1615
3 -10 -10 0.0801
3 -3 -13 0.0970

_exptl_crystal_preparation       
'Molybdenum pentachloride was dissolved in diethyl ether and cooled to -35 C. After cooling for approximately 10 minutes, allyltrimethylsilane was added to the solution which was then allowed to stir for 2 hours, during which the product precipitated as a red-orange powder.'
_exptl_crystal_recrystallization_method 
'The red-orange powder from the synthetic step was dissolved in a minimal amount of toluene and allowed to sit, unperturbed, in the glovebox freezer at -35 C overnight.'
_exptl_crystal_size_max          0.431
_exptl_crystal_size_mid          0.287
_exptl_crystal_size_min          0.147
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.5550 -10.2676 9.7765 -0.0000 -0.0256 0.9997
-0.0110 9.8310 9.7021 0.0000 0.9701 0.2425
1.5458 9.9474 -9.9722 -0.0000 0.0000 -1.0000
-0.1721 -11.2279 -8.7344 -0.0000 -0.9916 -0.1293
-10.5260 -2.7968 2.8464 -0.9572 -0.2035 0.2060
2.5279 9.9750 -10.0041 0.0927 0.0197 -0.9955
10.0676 5.0082 -5.0600 0.8811 0.1873 -0.4343
0.0186 -9.7240 9.7419 0.1451 0.0308 0.9889
7.9623 8.0497 -8.0982 0.6366 0.1353 -0.7593
-5.6706 -10.3401 -4.9175 -0.4997 -0.8654 0.0370
-8.9092 -7.1043 -1.1561 -0.8024 -0.5830 0.1280
6.8700 0.1912 7.0631 0.7032 0.5109 0.4945
7.4930 11.0742 -4.9801 0.5934 0.4311 -0.6798
5.9653 -5.4774 -11.2469 0.5218 -0.7182 -0.4603
2.6157 -14.8998 2.8285 0.3775 -0.5196 0.7665
-5.0604 -0.0267 12.4424 -0.3871 0.5327 0.7526
-7.5823 4.9363 10.3018 -0.6784 0.6108 0.4084
8.7623 -7.2285 1.4760 0.8949 -0.0941 0.4363
7.4613 10.9190 0.4706 0.6322 0.7021 -0.3278
3.1943 -9.9213 -9.9984 0.3005 -0.9248 -0.2334
3.1943 -2.5906 -12.5499 0.2282 -0.7023 -0.6743

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6900
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.612
_diffrn_reflns_theta_min         2.948
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.1(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00  -9.00   0.50    5.00    --   20.00  54.00 150.00  130
  2  ω     14.00  40.00   0.50    5.00    --   20.00  54.00 150.00   52
  3  ω    -25.00  31.00   0.50    5.00    --   20.00  54.00-150.00  112
  4  ω    -74.00  76.00   0.50    5.00    --   20.00  54.00 -60.00  300
  5  ω     -1.00  48.00   0.50    5.00    --   20.00  54.00-120.00   98
  6  ω     55.00  81.00   0.50    5.00    --   20.00  54.00-120.00   52
  7  ω    -46.00  53.00   0.50    5.00    --   20.00  54.00  60.00  198
  8  ω     48.00  73.00   0.50    5.00    --   20.00  54.00-180.00   50
  9  ω     28.00  54.00   0.50    5.00    --   20.00  54.00 -90.00   52
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0948812000
_diffrn_orient_matrix_UB_12      -0.0072611000
_diffrn_orient_matrix_UB_13      0.0074650000
_diffrn_orient_matrix_UB_21      0.0203771000
_diffrn_orient_matrix_UB_22      0.0481687000
_diffrn_orient_matrix_UB_23      0.0512072000
_diffrn_orient_matrix_UB_31      0.0077147000
_diffrn_orient_matrix_UB_32      -0.0380284000
_diffrn_orient_matrix_UB_33      0.0635407000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed 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                1935
_reflns_number_total             2234
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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         0.440
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.0173(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         2234
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0212
_refine_ls_restrained_S_all      1.068
_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)+(0.0209P)²+0.1730P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0516
_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:
 C3(H3A,H3B), C1(H1A,H1B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C)
;
_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 0.500000 0.500000 0.500000 0.02736(7) Uani 1 2 d S . P . .
Cl2 Cl 0.49923(7) 0.37294(4) 0.70574(5) 0.04666(12) Uani 1 1 d . . . . .
Cl1 Cl 0.18724(6) 0.46265(5) 0.37962(6) 0.04842(12) Uani 1 1 d . . . . .
O1 O 0.57174(15) 0.36245(10) 0.37996(13) 0.0346(3) Uani 1 1 d . . . . .
C3 C 0.4791(2) 0.24839(15) 0.3613(2) 0.0421(4) Uani 1 1 d . . . . .
H3A H 0.432109 0.230938 0.252041 0.051 Uiso 1 1 calc R U . . .
H3B H 0.375549 0.252435 0.404101 0.051 Uiso 1 1 calc R U . . .
C1 C 0.7190(2) 0.37180(16) 0.3026(2) 0.0416(4) Uani 1 1 d . . . . .
H1A H 0.809404 0.311399 0.341905 0.050 Uiso 1 1 calc R U . . .
H1B H 0.779559 0.446616 0.327496 0.050 Uiso 1 1 calc R U . . .
C2 C 0.6481(3) 0.3603(2) 0.1311(2) 0.0604(6) Uani 1 1 d . . . . .
H2A H 0.743330 0.380425 0.084763 0.091 Uiso 1 1 calc R U . . .
H2B H 0.545518 0.411728 0.093306 0.091 Uiso 1 1 calc R U . . .
H2C H 0.609810 0.281368 0.104987 0.091 Uiso 1 1 calc R U . . .
C4 C 0.6032(3) 0.15257(18) 0.4386(3) 0.0619(6) Uani 1 1 d . . . . .
H4A H 0.701331 0.144442 0.391592 0.093 Uiso 1 1 calc R U . . .
H4B H 0.535313 0.080979 0.427706 0.093 Uiso 1 1 calc R U . . .
H4C H 0.653001 0.170437 0.546245 0.093 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 Cl2 2.3611(4) 3_666 ?
Mo1 Cl2 2.3611(4) . ?
Mo1 Cl1 2.3567(4) . ?
Mo1 Cl1 2.3567(4) 3_666 ?
Mo1 O1 2.0716(11) . ?
Mo1 O1 2.0716(11) 3_666 ?
O1 C3 1.4728(18) . ?
O1 C1 1.4793(18) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.487(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.494(3) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
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
Cl2 Mo1 Cl2 180.0 . 3_666 ?
Cl1 Mo1 Cl2 88.588(18) . 3_666 ?
Cl1 Mo1 Cl2 88.589(18) 3_666 . ?
Cl1 Mo1 Cl2 91.411(18) 3_666 3_666 ?
Cl1 Mo1 Cl2 91.412(18) . . ?
Cl1 Mo1 Cl1 180.0 3_666 . ?
O1 Mo1 Cl2 89.98(3) 3_666 3_666 ?
O1 Mo1 Cl2 89.98(3) . . ?
O1 Mo1 Cl2 90.02(3) 3_666 . ?
O1 Mo1 Cl2 90.02(3) . 3_666 ?
O1 Mo1 Cl1 90.00(3) . 3_666 ?
O1 Mo1 Cl1 90.00(3) 3_666 . ?
O1 Mo1 Cl1 90.00(3) . . ?
O1 Mo1 Cl1 90.00(3) 3_666 3_666 ?
O1 Mo1 O1 180.00(5) . 3_666 ?
C3 O1 Mo1 123.31(9) . . ?
C3 O1 C1 114.25(12) . . ?
C1 O1 Mo1 122.43(10) . . ?
O1 C3 H3A 109.1 . . ?
O1 C3 H3B 109.1 . . ?
O1 C3 C4 112.58(15) . . ?
H3A C3 H3B 107.8 . . ?
C4 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
O1 C1 H1A 109.1 . . ?
O1 C1 H1B 109.1 . . ?
O1 C1 C2 112.46(15) . . ?
H1A C1 H1B 107.8 . . ?
C2 C1 H1A 109.1 . . ?
C2 C1 H1B 109.1 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 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
Mo1 O1 C3 C4 -115.53(16) . . . . ?
Mo1 O1 C1 C2 -115.22(15) . . . . ?
C3 O1 C1 C2 63.6(2) . . . . ?
C1 O1 C3 C4 65.7(2) . . . . ?


_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on the diffractometer using a MiteGen mount. '
_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 1.183
_oxdiff_exptl_absorpt_empirical_full_min 0.863
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sattelberger_05
_database_code_depnum_ccdc_archive 'CCDC 2151145'
loop_
_audit_author_name
_audit_author_address
'Thomas Shaw'
;University of Central Florida
United States of America
;
_audit_update_record             
;
2022-02-09 deposited with the CCDC.	2022-04-22 downloaded from the CCDC.
;
_audit_creation_date             2022-02-07
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        
Tetrachloro(1,2-dimethoxyethane)molybdenum(IV)
_chemical_formula_moiety         'C4 H10 Cl4 Mo O2'
_chemical_formula_sum            'C4 H10 Cl4 Mo O2'
_chemical_formula_weight         327.86
_chemical_absolute_configuration .
_chemical_melting_point          ?
_chemical_oxdiff_formula         MoCl4C3N1O1H7
_chemical_oxdiff_usercomment     'small 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'

_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           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   8.0686(5)
_cell_length_b                   11.3057(6)
_cell_length_c                   11.6997(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.519(5)
_cell_angle_gamma                90
_cell_volume                     1067.22(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8788
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      33.5510
_cell_measurement_theta_min      3.0770
_shelx_estimated_absorpt_T_max   0.972
_shelx_estimated_absorpt_T_min   0.464
_exptl_absorpt_coefficient_mu    2.185
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.106a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.041
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             640
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 1 -1 0.2652
2 -1 1 0.2582
0 -1 2 0.0481
0 1 -2 0.0181
0 1 0 0.0065
0 -1 0 0.0065

_exptl_crystal_recrystallization_method 
'Single crystals were obtained via a vapor diffusion technique. Tetrachlorobis(diethyl ether)molybdenum(IV) was dissolved in 1,2-dimethoxyethane and placed in a vapor diffusion vial set up with hexanes as the counter solvent. The crystallization was allowed to sit, unperturbed, for three days.'
_exptl_crystal_size_max          0.415
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.013
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.9974 1.0001 -1.0002 0.0472 -0.0868 0.1699
1.9974 -1.0001 1.0002 -0.0472 0.0868 -0.1699
-0.0000 -0.9992 1.9988 -0.1290 -0.0179 -0.0409
0.0000 0.9992 -1.9988 0.1290 0.0179 0.0409
0.0004 0.9991 0.0003 0.0406 -0.0463 -0.0118
-0.0004 -0.9991 -0.0003 -0.0406 0.0463 0.0118

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8141
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.102
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -2.00  86.00   0.50    2.00    --   13.12  57.00 -30.00  176
  2  ω     -9.00  86.00   0.50    2.00    --   13.12  77.00  90.00  190
  3  ω     -9.00  33.00   0.50    2.00    --   13.12  77.00 150.00   84
  4  ω     -2.00  86.00   0.50    2.00    --   13.12  57.00   0.00  176
  5  ω    -53.00  -3.00   0.50    2.00    --  -13.59 112.00  -2.00  100
  6  ω    -86.00 -39.00   0.50    2.00    --  -13.59 178.00  90.00   94
  7  ω    -86.00 -39.00   0.50    2.00    --  -13.59 178.00 -60.00   94
  8  ω    -62.00   5.00   0.50    2.00    --   13.12 -19.00   0.00  134
  9  ω    -62.00   5.00   0.50    2.00    --   13.12 -19.00  60.00  134
 10  ω    -62.00   5.00   0.50    2.00    --   13.12 -19.00 -60.00  134
 11  ω    -23.00  47.00   0.50    2.00    --   13.12 -99.00-150.00  140
 12  ω      3.00  54.00   0.50    2.00    --   13.12-112.00 -95.00  102
 13  ω     39.00  86.00   0.50    2.00    --   13.12-178.00   0.00   94
 14  ω     39.00  86.00   0.50    2.00    --   13.12-178.00  30.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0188355000
_diffrn_orient_matrix_UB_12      0.0406671000
_diffrn_orient_matrix_UB_13      -0.0441852000
_diffrn_orient_matrix_UB_21      0.0363429000
_diffrn_orient_matrix_UB_22      -0.0463050000
_diffrn_orient_matrix_UB_23      -0.0320915000
_diffrn_orient_matrix_UB_31      -0.0777649000
_diffrn_orient_matrix_UB_32      -0.0117883000
_diffrn_orient_matrix_UB_33      -0.0263752000
_diffrn_oxdiff_digest_frames     
;
014f53dc9381c410ab7b33948b4556502d01746ea7a
;
_diffrn_oxdiff_digest_hkl        
;
01c6ee0babc39b022fc7c5d925db979d82cc0c
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.894
_reflns_Friedel_fraction_full    0.912
_reflns_Friedel_fraction_max     0.900
_reflns_number_gt                1987
_reflns_number_total             2068
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.106a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details 
;
 Flack x determined using 843 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.12(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         2068
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0372
_refine_ls_restrained_S_all      1.165
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0712P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1093
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
1.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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 0.57198(7) 0.23444(5) 0.50224(6) 0.0134(2) Uani 1 1 d . . . . .
Cl1 Cl 0.5453(3) 0.14488(19) 0.32345(16) 0.0203(5) Uani 1 1 d . . . . .
Cl2 Cl 0.7216(4) 0.0799(2) 0.5799(2) 0.0329(6) Uani 1 1 d . . . . .
Cl3 Cl 0.8044(3) 0.3422(2) 0.4555(2) 0.0267(5) Uani 1 1 d . . . . .
Cl4 Cl 0.5359(3) 0.33067(17) 0.67651(16) 0.0185(5) Uani 1 1 d . . . . .
O1 O 0.3313(9) 0.1597(5) 0.5383(5) 0.0197(13) Uani 1 1 d . . . . .
O2 O 0.4030(7) 0.3647(5) 0.4344(5) 0.0145(12) Uani 1 1 d . . . . .
C1 C 0.3029(17) 0.0877(8) 0.6387(9) 0.032(3) Uani 1 1 d . . . . .
H1A H 0.390547 0.028003 0.645499 0.048 Uiso 1 1 calc GR . . . .
H1B H 0.195107 0.048248 0.631554 0.048 Uiso 1 1 calc GR . . . .
H1C H 0.303782 0.137967 0.706911 0.048 Uiso 1 1 calc GR . . . .
C2 C 0.1975(15) 0.2455(8) 0.5218(10) 0.024(2) Uani 1 1 d . . . . .
H2A H 0.189014 0.297689 0.589423 0.028 Uiso 1 1 calc R . . . .
H2B H 0.090364 0.204004 0.511094 0.028 Uiso 1 1 calc R . . . .
C3 C 0.2375(12) 0.3172(7) 0.4172(8) 0.0203(19) Uani 1 1 d . . . . .
H3A H 0.233734 0.266616 0.348114 0.024 Uiso 1 1 calc R . . . .
H3B H 0.156378 0.382172 0.407364 0.024 Uiso 1 1 calc R . . . .
C4 C 0.4444(11) 0.4502(8) 0.3471(7) 0.0188(18) Uani 1 1 d . . . . .
H4A H 0.551372 0.486862 0.365785 0.028 Uiso 1 1 calc GR . . . .
H4B H 0.358411 0.511364 0.343555 0.028 Uiso 1 1 calc GR . . . .
H4C H 0.451505 0.410418 0.272910 0.028 Uiso 1 1 calc GR . . . .


_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 2.3321(18) . ?
Mo1 Cl2 2.306(2) . ?
Mo1 Cl3 2.306(3) . ?
Mo1 Cl4 2.332(2) . ?
Mo1 O1 2.163(7) . ?
Mo1 O2 2.153(5) . ?
O1 C1 1.449(11) . ?
O1 C2 1.463(13) . ?
O2 C3 1.452(11) . ?
O2 C4 1.448(10) . ?
C2 C3 1.505(14) . ?

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 Cl1 93.90(8) . . ?
Cl2 Mo1 Cl3 94.01(10) . . ?
Cl2 Mo1 Cl4 94.48(8) . . ?
Cl3 Mo1 Cl1 94.88(9) . . ?
Cl3 Mo1 Cl4 93.97(8) . . ?
Cl4 Mo1 Cl1 167.35(9) . . ?
O1 Mo1 Cl1 85.99(17) . . ?
O1 Mo1 Cl2 95.45(18) . . ?
O1 Mo1 Cl3 170.42(17) . . ?
O1 Mo1 Cl4 83.80(17) . . ?
O2 Mo1 Cl1 85.02(16) . . ?
O2 Mo1 Cl2 172.28(18) . . ?
O2 Mo1 Cl3 93.70(16) . . ?
O2 Mo1 Cl4 85.41(16) . . ?
O2 Mo1 O1 76.9(2) . . ?
C1 O1 Mo1 121.8(7) . . ?
C1 O1 C2 111.0(8) . . ?
C2 O1 Mo1 112.2(5) . . ?
C3 O2 Mo1 112.1(5) . . ?
C4 O2 Mo1 124.6(5) . . ?
C4 O2 C3 111.6(7) . . ?
O1 C2 C3 107.5(9) . . ?
O2 C3 C2 106.9(8) . . ?


_olex2_date_sample_data_collection 2021-04-21
_olex2_date_sample_submission    2021-04-15
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder with Paratone oil'
_olex2_submission_original_sample_id Sattelberger_05
_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 4.428
_oxdiff_exptl_absorpt_empirical_full_min 0.562
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
