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_7246971
_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         'C17 H19 Mo O2 S2, B F4'
_chemical_formula_sum            'C17 H19 B F4 Mo O2 S2'
_chemical_formula_weight         502.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 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                 105.9450(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.94230(10)
_cell_length_b                   12.29590(10)
_cell_length_c                   23.7796(2)
_cell_measurement_reflns_used    53801
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.3790
_cell_measurement_theta_min      3.2680
_cell_volume                     3919.77(6)
_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      100.00(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     35.00 123.00   0.50    0.12    --   47.70  19.00   0.00  176
  2  \w     99.00 127.00   0.50    0.49    --  107.74  57.00 -90.00   56
  3  \w    130.00 177.00   0.50    0.49    --  107.74  57.00 -90.00   94
  4  \w    149.00 178.00   0.50    0.49    --  107.74  57.00-150.00   58
  5  \w    143.00 175.00   0.50    0.49    --  107.74  69.00 -54.54   64
  6  \w    142.00 176.00   0.50    0.49    --  107.74  77.00   0.00   68
  7  \w     96.00 178.00   0.50    0.49    --  107.74 124.00 -96.00  164
  8  \w    103.00 171.00   0.50    0.49    --  107.74  77.00  30.00  136
  9  \w    104.00 137.00   0.50    0.49    --  107.74  77.00   0.00   66
 10  \w     95.00 172.00   0.50    0.49    --  107.74  57.00 -60.00  154
 11  \w     91.00 167.00   0.50    0.49    --  107.74  65.00  88.92  152
 12  \w     99.00 147.00   0.50    0.49    --  107.74  37.00 150.00   96
 13  \w     93.00 178.00   0.50    0.49    --  107.74  57.00  60.00  170
 14  \w     90.00 128.00   0.50    0.49    --  107.74  69.00 -54.54   76
 15  \w     95.00 175.00   0.50    0.49    --  107.74  57.00-120.00  160
 16  \w     95.00 176.00   0.50    0.49    --  107.74  37.00-180.00  162
 17  \w     95.00 137.00   0.50    0.49    --  107.74  57.00-150.00   84
 18  \w     92.00 175.00   0.50    0.49    --  107.74  68.00 -14.73  166
 19  \w     81.00 169.00   0.50    0.49    --  107.74 146.00  69.00  176
 20  \w     35.00 121.00   0.50    0.12    --   47.70  37.00-180.00  172
 21  \w     77.00 104.00   0.50    0.49    --  107.74 -77.00-180.00   54
 22  \w     34.00  95.00   0.50    0.12    --   47.70-124.00-176.00  122
 23  \w     35.00 111.00   0.50    0.49    --  107.74-124.00-176.00  152
 24  \w     49.00 111.00   0.50    0.49    --  107.74-125.00 -60.00  124
 25  \w     46.00 108.00   0.50    0.12    --   47.70-146.00  18.00  124
 26  \w     46.00 127.00   0.50    0.49    --  107.74-146.00  18.00  162
 27  \w     82.00 107.00   0.50    0.49    --  107.74-106.00 124.22   50
 28  \w     38.00 111.00   0.50    0.49    --  107.74-125.00 150.00  146
 29  \w     38.00 111.00   0.50    0.49    --  107.74-125.00  30.00  146
 30  \w     35.00  60.00   0.50    0.49    --  107.74-106.00 124.22   50
 31  \w     35.00 102.00   0.50    0.49    --  107.74 -99.00  60.00  134
 32  \w     36.00  92.00   0.50    0.49    --  107.74 -99.00  30.00  112
 33  \w     37.00  64.00   0.50    0.49    --  107.74 -57.00 -60.00   54
 34  \w     40.00  96.00   0.50    0.49    --  107.74 -77.00 -90.00  112
 35  \w     36.00 102.00   0.50    0.49    --  107.74 -99.00-150.00  132
 36  \w     36.00  70.00   0.50    0.49    --  107.74 -77.00-180.00   68
 37  \w     31.00 120.00   0.50    0.12    --   47.70  63.00-140.97  178
 38  \w     33.00 120.00   0.50    0.12    --   47.70  57.00-180.00  174
 39  \w     31.00 120.00   0.50    0.12    --   47.70  61.00-114.42  178
 40  \w     35.00 121.00   0.50    0.12    --   47.70  37.00  60.00  172
 41  \w     33.00 120.00   0.50    0.12    --   47.70  57.00  30.00  174
 42  \w     30.00 120.00   0.50    0.12    --   47.70  64.00 -87.74  180
 43  \w     30.00 120.00   0.50    0.12    --   47.70  64.00 -54.65  180
 44  \w     33.00 120.00   0.50    0.12    --   47.70  57.00-159.12  174
 45  \w     33.00 120.00   0.50    0.12    --   47.70  57.00   0.00  174
 46  \w     33.00 120.00   0.50    0.12    --   47.70  57.00  90.00  174
 47  \w     33.00  59.00   0.50    0.12    --   47.70  57.00  60.00   52
 48  \w     35.00  65.00   0.50    0.49    --  107.74 -57.00 150.00   60
 49  \w    -86.00 -12.00   0.50    0.12    --  -47.70 124.00 -96.00  148
 50  \w    -85.00 -13.00   0.50    0.49    --  -86.25 124.00 -96.00  144
 51  \w    -87.00 -62.00   0.50    0.49    --  -86.25 146.00  69.00   50
 52  \w   -101.00 -24.00   0.50    0.12    --  -47.70 146.00  69.00  154
 53  \w   -119.00 -33.00   0.50    0.12    --  -47.70 -57.00  60.00  172
 54  \w    -94.00 -69.00   0.50    0.49    --  -86.25 -63.00 -75.30   50
 55  \w    -99.00 -69.00   0.50    0.49    --  -86.25 -62.00 -36.97   60
 56  \w    -95.00 -69.00   0.50    0.49    --  -86.25 -62.00 -25.06   52
 57  \w    -96.00 -71.00   0.50    0.49    --  -86.25 -62.00 -82.80   50
 58  \w   -102.00 -72.00   0.50    0.49    --  -86.25 -64.00-116.63   60
 59  \w   -103.00 -69.00   0.50    0.49    --  -86.25 -62.00-135.68   68
 60  \w    -95.00 -69.00   0.50    0.49    --  -86.25 -63.00-168.95   52
 61  \w    -97.00 -71.00   0.50    0.49    --  -86.25 -62.00-157.42   52
 62  \w    -96.00 -71.00   0.50    0.49    --  -86.25 -57.00-120.00   50
 63  \w    -99.00 -72.00   0.50    0.49    --  -86.25 -53.00 -75.32   54
 64  \w    -95.00 -69.00   0.50    0.49    --  -86.25 -62.00 -92.17   52
 65  \w    -96.00 -71.00   0.50    0.49    --  -86.25 -57.00 -60.00   50
 66  \w    -98.00 -72.00   0.50    0.49    --  -86.25 -64.00  -1.24   52
 67  \w    -94.00 -69.00   0.50    0.49    --  -86.25 -63.00  15.86   50
 68  \w    -96.00 -71.00   0.50    0.49    --  -86.25 -57.00  52.97   50
 69  \w    -97.00 -69.00   0.50    0.49    --  -86.25 -63.00 107.14   56
 70  \w    -98.00 -69.00   0.50    0.49    --  -86.25 -63.00 148.07   58
 71  \w    -95.00 -70.00   0.50    0.49    --  -86.25 -60.00 172.58   50
 72  \w    -94.00 -69.00   0.50    0.49    --  -86.25 -63.00 158.35   50
 73  \w   -109.00 -71.00   0.50    0.49    --  -86.25 -57.00 120.00   76
 74  \w   -104.00 -69.00   0.50    0.49    --  -86.25 -63.00  81.91   70
 75  \w    -96.00 -70.00   0.50    0.49    --  -86.25 -61.00  46.39   52
 76  \w    -98.00 -72.00   0.50    0.49    --  -86.25 -64.00  -8.60   52
 77  \w   -102.00 -72.00   0.50    0.49    --  -86.25 -64.00  40.05   60
 78  \w   -103.00 -70.00   0.50    0.49    --  -86.25 -60.00  82.51   66
 79  \w   -107.00 -70.00   0.50    0.49    --  -86.25 -60.00  25.65   74
 80  \w   -119.00 -30.00   0.50    0.12    --  -47.70 -63.00  48.55  178
 81  \w    -97.00 -70.00   0.50    0.49    --  -86.25 -63.00-100.02   54
 82  \w    -96.00 -70.00   0.50    0.49    --  -86.25 -62.00-139.62   52
 83  \w   -119.00 -33.00   0.50    0.12    --  -47.70 -57.00-120.00  172
 84  \w   -115.00 -69.00   0.50    0.49    --  -86.25 -62.00  -1.67   92
 85  \w   -119.00 -33.00   0.50    0.12    --  -47.70 -57.00  90.00  172
 86  \w   -110.00 -69.00   0.50    0.49    --  -86.25 -62.00 132.85   82
 87  \w   -119.00 -35.00   0.50    0.12    --  -47.70 -47.00  97.94  168
 88  \w   -119.00 -59.00   0.50    0.12    --  -47.70-146.00  18.00  120
 89  \w   -140.00-114.00   0.50    0.49    --  -86.25 -62.00 132.85   52
 90  \w   -141.00-115.00   0.50    0.49    --  -86.25 -60.00 172.58   52
 91  \w   -157.00-132.00   0.50    0.49    --  -86.25 -60.00  82.51   50
 92  \w   -156.00-130.00   0.50    0.49    --  -86.25 -60.00  25.65   52
 93  \w   -159.00-115.00   0.50    0.49    --  -86.25 -63.00  15.86   88
 94  \w   -146.00-120.00   0.50    0.49    --  -86.25 -57.00 -60.00   52
 95  \w   -158.00-114.00   0.50    0.49    --  -86.25 -62.00-139.62   88
 96  \w   -140.00-114.00   0.50    0.49    --  -86.25 -62.00-135.68   52
 97  \w   -156.00-130.00   0.50    0.49    --  -86.25 -64.00-116.63   52
 98  \w   -159.00-133.00   0.50    0.49    --  -86.25 -63.00 -75.30   52
 99  \w   -159.00-123.00   0.50    0.49    --  -86.25 -62.00 -82.80   72
100  \w   -158.00-132.00   0.50    0.49    --  -86.25 -62.00-157.42   52
101  \w   -158.00-131.00   0.50    0.49    --  -86.25 -63.00-100.02   54
102  \w   -159.00 -74.00   0.50    0.49    --  -86.25-124.00-176.00  170
103  \w   -152.00 -59.00   0.50    0.49    --  -86.25-146.00  18.00  186
;
_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      -0.0253995000
_diffrn_orient_matrix_UB_12      -0.0865394000
_diffrn_orient_matrix_UB_13      -0.0486850000
_diffrn_orient_matrix_UB_21      -0.0319831000
_diffrn_orient_matrix_UB_22      0.0903448000
_diffrn_orient_matrix_UB_23      -0.0462389000
_diffrn_orient_matrix_UB_31      0.1074580000
_diffrn_orient_matrix_UB_32      0.0063779000
_diffrn_orient_matrix_UB_33      -0.0054700000
_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  0.0520
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            66765
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.584
_diffrn_reflns_theta_max         66.584
_diffrn_reflns_theta_min         3.867
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.903
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.521
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_description       prism
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0195
_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^)+(0.0282P)^2^+6.2526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0519
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3457
_reflns_number_total             3467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra03383j2.cif
_cod_data_source_block           jv201113mo1_cu_100k-gg
_cod_database_code               7246971
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C12 H11 Mo S1 O5 F3 '
_shelx_estimated_absorpt_t_max   0.648
_shelx_estimated_absorpt_t_min   0.216
_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 Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C8(H8a,H8b)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C11(H11), C14(H14), C4(H4), C7(H7), C5(H5), C13(H13), C6(H6),
 C12(H12)
2.c Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C16(H16a,H16b,H16c)
;
_shelx_res_checksum              16808
_shelx_hkl_checksum              72272
_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 2.321
_oxdiff_exptl_absorpt_empirical_full_min 0.547