Stabilization of propene molybdenum and tungsten half–sandwich complexes by intramolecular coordination of a thioether function
Hanzl, Lukáš; Vinklárek, Jaromír; Dostál, Libor; Císařová, Ivana; Litecká, Miroslava; Honzíček, Jan; RSC Advances 13 (2023) 19746–19756; doi:10.1039/D3RA03383J

data_7246966
_publ_section_title
;
 Stabilization of propene molybdenum and tungsten half--sandwich complexes
 by intramolecular coordination of a thioether function
;
_journal_issue                   29
_journal_name_full               'RSC Advances'
_journal_page_first              19746
_journal_page_last               19756
_journal_paper_doi               10.1039/D3RA03383J
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C15 H21 Mo O2 S2, B F4'
_chemical_formula_sum            'C15 H21 B F4 Mo O2 S2'
_chemical_formula_weight         480.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-25
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2023-02-24 deposited with the CCDC.	2023-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.8780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.24110(10)
_cell_length_b                   12.0733(2)
_cell_length_c                   18.5383(3)
_cell_measurement_reflns_used    12516
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      77.2970
_cell_measurement_theta_min      4.3750
_cell_volume                     1837.83(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_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    -25.00  27.00   0.50    0.05    --  -47.70  19.00 -30.00  104
  2  \w     -2.00  28.00   0.50    0.05    --  -47.70  19.00-150.00   60
  3  \w    -42.00 -14.00   0.50    0.17    --  -86.25  37.00 -30.00   56
  4  \w    -39.00 -13.00   0.50    0.17    --  -86.25  37.00   0.00   52
  5  \w    -41.00 -13.00   0.50    0.17    --  -86.25  37.00  60.00   56
  6  \w    -91.00 -17.00   0.50    0.05    --  -47.70 132.00  13.00  148
  7  \w    -85.00 -14.00   0.50    0.17    --  -86.25 125.00   0.00  142
  8  \w    -94.00 -19.00   0.50    0.05    --  -47.70 136.00-169.00  150
  9  \w    -26.00  13.00   0.50    0.05    --   47.70 -19.00-150.00   78
 10  \w     61.00  87.00   0.50    0.17    --  107.74 -77.00-180.00   52
 11  \w     47.00  72.00   0.50    0.17    --  107.74-125.00-180.00   50
 12  \w     85.00 111.00   0.50    0.17    --  107.74-125.00-180.00   52
 13  \w     38.00  99.00   0.50    0.05    --   47.70-132.00 -56.00  122
 14  \w     38.00 117.00   0.50    0.17    --  107.74-132.00 -56.00  158
 15  \w     35.00  60.00   0.50    0.17    --  107.74 -57.00  60.00   50
 16  \w     36.00  66.00   0.50    0.17    --  107.74 -57.00   0.00   60
 17  \w     41.00 101.00   0.50    0.05    --   47.70-136.00 126.00  120
 18  \w     72.00 119.00   0.50    0.17    --  107.74-136.00 126.00   94
 19  \w     41.00 103.00   0.50    0.17    --  107.74 -77.00 150.00  124
 20  \w     35.00  92.00   0.50    0.17    --  107.74 -77.00 120.00  114
 21  \w    128.00 177.00   0.50    0.17    --  107.74  37.00 -60.00   98
 22  \w     97.00 178.00   0.50    0.17    --  107.74  57.00   0.00  162
 23  \w     95.00 125.00   0.50    0.17    --  107.74  37.00 -60.00   60
 24  \w     88.00 175.00   0.50    0.17    --  107.74 136.00-169.00  174
 25  \w    -94.00 -19.00   0.50    0.17    --  -86.25 136.00-169.00  150
 26  \w   -119.00 -69.00   0.50    0.05    --  -47.70-132.00 -56.00  100
 27  \w   -118.00 -74.00   0.50    0.05    --  -47.70-125.00-180.00   88
 28  \w   -159.00 -69.00   0.50    0.17    --  -86.25-132.00 -56.00  180
 29  \w   -119.00 -66.00   0.50    0.05    --  -47.70-136.00 126.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0388815000
_diffrn_orient_matrix_UB_12      0.1188093000
_diffrn_orient_matrix_UB_13      -0.0264676000
_diffrn_orient_matrix_UB_21      -0.0918420000
_diffrn_orient_matrix_UB_22      -0.0466318000
_diffrn_orient_matrix_UB_23      -0.0692732000
_diffrn_orient_matrix_UB_31      -0.1589031000
_diffrn_orient_matrix_UB_32      -0.0020024000
_diffrn_orient_matrix_UB_33      0.0381127000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17067
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         4.375
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.389
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.446
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_description       irregular
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0294P)^2^+0.9189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3083
_reflns_number_total             3249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra03383j2.cif
_cod_data_source_block           jv201027mo1_10_cu_100k-gg
_cod_database_code               7246966
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C15 H21 Mo S2 O2 B F4'
_chemical_oxdiff_usercomment     'store in inert, 2 crystal'
_shelx_estimated_absorpt_t_max   0.553
_shelx_estimated_absorpt_t_min   0.330
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C15(H15A,H15B), C11(H11A,H11B), C9(H9A,H9B), C10(H10A,H10B),
 C8(H8A,H8B), C14(H14A,H14B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C3(H3), C6(H6), C4(H4)
;
_shelx_res_checksum              1433
_shelx_hkl_checksum              26443
_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 4.175
_oxdiff_exptl_absorpt_empirical_full_min 0.410