Synthesis, properties and structural features of molybdenum(v) oxide trichloride complexes with neutral chalcogenoether ligands.
Smith, Danielle E.; Levason, William; Powell, James; Reid, Gillian; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4380–4389; doi:10.1039/d1dt00038a

data_7706762
_publ_section_title
;
 Synthesis, properties and structural features of molybdenum(v) oxide
 trichloride complexes with neutral chalcogenoether ligands.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4380
_journal_page_last               4389
_journal_paper_doi               10.1039/d1dt00038a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C4 H12 Cl6 Mo2 O2 S2'
_chemical_formula_sum            'C4 H12 Cl6 Mo2 O2 S2'
_chemical_formula_weight         560.84
_chemical_name_systematic        '[MoOCl2(SMe)2)(Cl)2]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-05-04
_audit_creation_method
;
Olex2 1.3
(compiled Sep 10 2019 10:52:38 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-12-16 deposited with the CCDC.	2021-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.1720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.81110(10)
_cell_length_b                   9.50630(10)
_cell_length_c                   11.2487(2)
_cell_measurement_reflns_used    18670
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.7760
_cell_measurement_theta_min      2.8270
_cell_volume                     806.15(2)
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -98.00  22.00   0.50    0.50    --   -8.30 -60.00-150.00  240
  2  \w    -98.00  22.00   0.50    0.50    --   -8.30 -60.00 -30.00  240
  3  \w    -98.00  21.00   0.50    0.50    --   -8.30 -57.00  60.00  238
  4  \w    -98.00  81.00   0.50    0.50    --   -8.30   0.00-180.00  358
  5  \w    -39.00  32.00   0.50    0.50    --   -8.30  60.00  30.00  142
  6  \w    -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       '\w 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_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_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_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_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.310
_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
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.064
_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_restrained_S_all      1.208
_refine_ls_R_factor_all          0.0122
_refine_ls_R_factor_gt           0.0119
_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/[\s^2^(Fo^2^)+(0.0094P)^2^+0.3552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0276
_refine_ls_wR_factor_ref         0.0277
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2654
_reflns_number_total             2693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00038a2.cif
_cod_data_source_block           moocl3(sme2)2-1
_cod_depositor_comments
'Adding full bibliography for 7706761--7706769.cif.'
_cod_database_code               7706762
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         MoOCl3S2C4H12
_chemical_oxdiff_usercomment     'Dark Green Block'
_shelx_estimated_absorpt_t_max   0.488
_shelx_estimated_absorpt_t_min   0.401
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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)
;
_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