Synthesis, Characterization, X-ray and Electronic Structures of Diethyl Ether and 1,2-Dimethoxyethane Adducts of Molybdenum(IV) Chloride and Tungsten(IV) Chloride
Shaw, Thomas E.; Diethrich, Timothy J. J.; Stern, Charlotte L.; Scott, Brian; Jurca, Titel; Gilbert, Thomas M.; Sattelberger, Alfred P.; Dalton Transactions  (2022) –; doi:10.1039/D2DT00787H

data_7710167
_publ_section_title
;
 Synthesis, Characterization, X-ray and Electronic Structures of Diethyl
 Ether and 1,2-Dimethoxyethane Adducts of Molybdenum(IV) Chloride and
 Tungsten(IV) Chloride
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00787H
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C4 H10 Cl4 O2 W'
_chemical_formula_sum            'C4 H10 Cl4 O2 W'
_chemical_formula_weight         415.77
_chemical_name_systematic        Tetrachloro(1,2-dimethoxyethane)tungsten(IV)
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-02-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-09 deposited with the CCDC.	2022-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.687(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0766(2)
_cell_length_b                   11.3089(2)
_cell_length_c                   11.7413(3)
_cell_measurement_reflns_used    16956
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      33.8020
_cell_measurement_theta_min      3.0780
_cell_volume                     1072.34(4)
_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)'
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -2.00  42.00   0.50   19.82    --   13.12  85.00  25.00   88
  2  \w     14.00  40.00   0.50   19.82    --   13.12 -85.00 -93.00   52
  3  \w    -41.00  -2.00   0.50   19.82    --  -13.59 -85.00 -93.00   78
  4  \w    -40.00   6.00   0.50   19.82    --  -13.59  85.00  25.00   92
  5  \w      2.00  80.00   0.50   19.82    --   13.12  37.00-180.00  156
  6  \w    -23.00   3.00   0.50   19.82    --   13.12 -99.00-120.00   52
  7  \w    -58.00   5.00   0.50   19.82    --   13.12 -19.00   0.00  126
  8  \w    -60.00   4.00   0.50   19.82    --   13.12 -19.00  60.00  128
  9  \w    -22.00  47.00   0.50   19.82    --   13.12 -99.00 150.00  138
 10  \w     22.00  47.00   0.50   19.82    --   13.12 -99.00-120.00   50
 11  \w     -2.00  75.00   0.50   19.82    --   13.12  57.00-150.00  154
 12  \w    -42.00   3.00   0.50   19.82    --   13.12 -19.00-180.00   90
 13  \w    -20.00   6.00   0.50   19.82    --   13.12 -99.00  60.00   52
 14  \w     18.00  47.00   0.50   19.82    --   13.12 -99.00  60.00   58
 15  \w     28.00  54.00   0.50   19.82    --   13.12-112.00-138.69   52
 16  \w    -77.00 -37.00   0.50   19.82    --  -13.59 -37.00-150.00   80
 17  \w    -82.00   1.00   0.50   19.82    --  -13.59 -57.00 -60.00  166
 18  \w    -26.00  60.00   0.50   19.82    --  -13.59  37.00 -60.00  172
 19  \w    -54.00 -29.00   0.50   19.82    --  -13.59 111.00 -87.30   50
 20  \w    -34.00  -3.00   0.50   19.82    --  -13.59 -37.00-150.00   62
 21  \w    -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       '\w 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_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_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_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.575
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_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
_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_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_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0224
_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/[\s^2^(Fo^2^)+(0.0350P)^2^+1.1463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0558
_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_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00787h2.cif
_cod_data_source_block           sattelberger_04
_cod_database_code               7710167
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         WCl4CNO
_shelx_estimated_absorpt_t_max   0.799
_shelx_estimated_absorpt_t_min   0.555
_diffrn_oxdiff_digest_frames
;
01697f635f62e1e179d1b1a2f7f0edc182020362e7b
;
_diffrn_oxdiff_digest_hkl
;
01fa466dd2f53ebea48edc0a2f69b8737ac4ea
;
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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)
;
_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