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_7706764
_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         'C8 H18 Cl3 Mo O S2'
_chemical_formula_sum            'C8 H18 Cl3 Mo O S2'
_chemical_formula_weight         396.63
_chemical_name_systematic        '[MoOCl3(PrS(CH2)2SPr)]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.4629(2)
_cell_length_b                   13.7526(2)
_cell_length_c                   17.5032(6)
_cell_measurement_reflns_used    24989
_cell_measurement_temperature    112(17)
_cell_measurement_theta_max      31.0600
_cell_measurement_theta_min      3.1650
_cell_volume                     3000.00(12)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      112(17)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.898
_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    -35.00  77.00   1.00   23.72    --  -12.00  38.00 150.00  112
  2  \w   -101.00  17.00   1.00   23.72    --  -12.00 -60.00-120.00  118
  3  \w   -101.00  17.00   1.00   23.72    --  -12.00 -60.00  30.00  118
  4  \w   -101.00  17.00   1.00   23.72    --  -12.00 -60.00 150.00  118
  5  \w    -35.00  77.00   1.00   23.72    --  -12.00  38.00 -60.00  112
  6  \w    -41.00  77.00   1.00   23.72    --  -12.00  57.00  60.00  118
  7  \w    -41.00  77.00   1.00   23.72    --  -12.00  60.00 -30.00  118
  8  \w    -41.00 -16.00   1.00   23.72    --  -12.00  60.00 120.00   25
  9  \w    -41.00  77.00   1.00   23.72    --  -12.00  57.00-150.00  118
;
_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      -0.0021395000
_diffrn_orient_matrix_UB_12      -0.0009707000
_diffrn_orient_matrix_UB_13      -0.0404783000
_diffrn_orient_matrix_UB_21      0.0008917000
_diffrn_orient_matrix_UB_22      -0.0515666000
_diffrn_orient_matrix_UB_23      0.0007431000
_diffrn_orient_matrix_UB_31      -0.0568754000
_diffrn_orient_matrix_UB_32      -0.0007727000
_diffrn_orient_matrix_UB_33      0.0014891000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24043
_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         31.354
_diffrn_reflns_theta_min         3.183
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.662
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71882
_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 yellow'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_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          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.324
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         4429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+2.8238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3643
_reflns_number_total             4429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00038a2.cif
_cod_data_source_block           moocl3(prs(ch2)2spr)-3
_cod_depositor_comments
'Adding full bibliography for 7706761--7706769.cif.'
_cod_database_code               7706764
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo O S2 C H Cl'
_chemical_oxdiff_usercomment     DL-meth_DAC_Pr
_shelx_estimated_absorpt_t_max   0.732
_shelx_estimated_absorpt_t_min   0.635
_reflns_odcompleteness_completeness 97.67
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C3(H3A,H3B,H3C)
;
_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 2.509
_oxdiff_exptl_absorpt_empirical_full_min 0.532