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_7710169
_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_formula_moiety         'C4 H10 Cl4 Mo O2'
_chemical_formula_sum            'C4 H10 Cl4 Mo O2'
_chemical_formula_weight         327.86
_chemical_name_systematic        Tetrachloro(1,2-dimethoxyethane)molybdenum(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             2022-02-07
_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                 90.519(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0686(5)
_cell_length_b                   11.3057(6)
_cell_length_c                   11.6997(6)
_cell_measurement_reflns_used    8788
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      33.5510
_cell_measurement_theta_min      3.0770
_cell_volume                     1067.22(10)
_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)'
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -2.00  86.00   0.50    2.00    --   13.12  57.00 -30.00  176
  2  \w     -9.00  86.00   0.50    2.00    --   13.12  77.00  90.00  190
  3  \w     -9.00  33.00   0.50    2.00    --   13.12  77.00 150.00   84
  4  \w     -2.00  86.00   0.50    2.00    --   13.12  57.00   0.00  176
  5  \w    -53.00  -3.00   0.50    2.00    --  -13.59 112.00  -2.00  100
  6  \w    -86.00 -39.00   0.50    2.00    --  -13.59 178.00  90.00   94
  7  \w    -86.00 -39.00   0.50    2.00    --  -13.59 178.00 -60.00   94
  8  \w    -62.00   5.00   0.50    2.00    --   13.12 -19.00   0.00  134
  9  \w    -62.00   5.00   0.50    2.00    --   13.12 -19.00  60.00  134
 10  \w    -62.00   5.00   0.50    2.00    --   13.12 -19.00 -60.00  134
 11  \w    -23.00  47.00   0.50    2.00    --   13.12 -99.00-150.00  140
 12  \w      3.00  54.00   0.50    2.00    --   13.12-112.00 -95.00  102
 13  \w     39.00  86.00   0.50    2.00    --   13.12-178.00   0.00   94
 14  \w     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       '\w 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_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_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_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.041
_exptl_crystal_description       needle
_exptl_crystal_F_000             640
_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
_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_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_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0712P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1093
_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_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00787h2.cif
_cod_data_source_block           sattelberger_05
_cod_database_code               7710169
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         MoCl4C3N1O1H7
_chemical_oxdiff_usercomment     'small block'
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.464
_diffrn_oxdiff_digest_frames
;
014f53dc9381c410ab7b33948b4556502d01746ea7a
;
_diffrn_oxdiff_digest_hkl
;
01c6ee0babc39b022fc7c5d925db979d82cc0c
;
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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)
;
_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