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_7706769
_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         'C14 H14 Cl3 Mo O S2'
_chemical_formula_sum            'C14 H14 Cl3 Mo O S2'
_chemical_formula_weight         464.66
_chemical_name_systematic        '[MoOCl3(PhS(CH2)2SPh)]'
_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
_audit_creation_date             2020-06-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-16 deposited with the CCDC.	2021-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.1600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6139(2)
_cell_length_b                   6.80640(10)
_cell_length_c                   12.9677(2)
_cell_measurement_reflns_used    43730
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.9380
_cell_measurement_theta_min      2.1980
_cell_volume                     1721.19(4)
_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)'
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -98.00  21.00   0.50    0.50    --   -8.30 -57.00 -30.00  238
  2  \w    -98.00  22.00   0.50    0.50    --   -8.30 -60.00  90.00  240
  3  \w    -98.00  81.00   0.50    0.50    --   -8.30   0.00-150.00  358
  4  \w    -98.00  21.00   0.50    0.50    --   -8.30 -57.00-120.00  238
  5  \w    -39.00  81.00   0.50    0.50    --   -8.30  60.00 -90.00  240
  6  \w    -39.00  81.00   0.50    0.50    --   -8.30  60.00  60.00  240
  7  \w    -39.00  81.00   0.50    0.50    --   -8.30  60.00-180.00  240
  8  \w    -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       '\w 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_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_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_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_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_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.793
_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
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.121
_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_restrained_S_all      1.472
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0542
_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^)+7.6691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5485
_reflns_number_total             5833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00038a2.cif
_cod_data_source_block           moocl3(phs(ch2)2sph)
_cod_depositor_comments
'Adding full bibliography for 7706761--7706769.cif.'
_cod_database_code               7706769
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         MoOCl3S2C14H14
_chemical_oxdiff_usercomment     'Orange Block'
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.668
_diffrn_oxdiff_digest_frames
;
01614156ee8d529e13a1e93bdff17fdd73000564394
;
_diffrn_oxdiff_digest_hkl
;
01858ed693473f774e39cf6b517cd863a236f1
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_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)
;
_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