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_7246970
_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 O3 S2, B F4, 0.785(Cl), C0.5 H Cl0.215'
_chemical_formula_sum            'C15.5 H22 B Cl F4 Mo O3 S2'
_chemical_formula_weight         538.65
_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     direct
_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                 99.9370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.40920(10)
_cell_length_b                   17.28130(10)
_cell_length_c                   16.20890(10)
_cell_measurement_reflns_used    43523
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      77.1740
_cell_measurement_theta_min      3.7370
_cell_volume                     2044.26(3)
_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    'SHELXS  (Sheldrick, 2008)'
_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 0.989
_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    -54.00  -5.00   0.50    0.30    --  -47.70  57.00 -60.00   98
  2  \w    -42.00 -16.00   0.50    0.30    --    6.00 125.00 -49.44   52
  3  \w     -9.00  21.00   0.50    0.30    --   22.00  96.00 -78.15   60
  4  \w     10.00  40.00   0.50    0.30    --   38.00  91.00 -26.31   60
  5  \w     30.00  55.00   0.50    0.30    --   54.00  79.00 -40.19   50
  6  \w     71.00  97.00   0.50    0.30    --   54.00  79.00 -40.19   52
  7  \w     63.00  90.00   0.50    0.30    --   50.00  77.00  17.08   54
  8  \w     98.00 123.00   0.50    0.30    --   54.00  79.00  73.40   50
  9  \w    121.00 146.00   0.50    0.30    --   74.00  77.00  52.31   50
 10  \w    106.00 178.00   0.50    1.20    --  107.74 103.00 -28.00  144
 11  \w    149.00 177.00   0.50    1.20    --  107.74  37.00  60.00   56
 12  \w    126.00 178.00   0.50    1.20    --  107.74   0.00  60.00  104
 13  \w    101.00 126.00   0.50    0.30    --   54.00  72.00 166.18   50
 14  \w     77.00 103.00   0.50    0.30    --   54.00  76.00 126.30   52
 15  \w     49.00  75.00   0.50    0.30    --   70.00  75.00 168.25   52
 16  \w     42.00  68.00   0.50    0.30    --   54.00  72.00 166.18   52
 17  \w     43.00  68.00   0.50    0.30    --   66.00  77.00 121.39   50
 18  \w     38.00  63.00   0.50    0.30    --   62.00  80.00  96.04   50
 19  \w     51.00  77.00   0.50    0.30    --   74.00  77.00  79.40   52
 20  \w     51.00  77.00   0.50    0.30    --   74.00  77.00  52.31   52
 21  \w     53.00  79.00   0.50    0.30    --   74.00  75.00  32.56   52
 22  \w     37.00  63.00   0.50    0.30    --   58.00  78.00 -43.12   52
 23  \w     27.00  57.00   0.50    0.30    --   50.00  77.00  17.08   60
 24  \w     31.00  57.00   0.50    0.30    --   54.00  77.00  44.93   52
 25  \w     30.00  57.00   0.50    0.30    --   54.00  79.00  73.40   54
 26  \w     33.00  59.00   0.50    0.30    --   54.00  76.00 126.30   52
 27  \w     17.00  42.00   0.50    0.30    --   46.00  90.00 126.35   50
 28  \w      8.00  33.00   0.50    0.30    --   38.00  93.00 178.85   50
 29  \w     -8.00  17.00   0.50    0.30    --   26.00 100.00 111.87   50
 30  \w     13.00  38.00   0.50    0.30    --   42.00  90.00  39.87   50
 31  \w     30.00  56.00   0.50    0.30    --   54.00  80.00 -99.61   52
 32  \w     47.00  75.00   0.50    0.30    --   70.00  78.00-122.44   56
 33  \w     31.00  80.00   0.50    0.30    --   54.00  78.00-126.67   98
 34  \w    111.00 136.00   0.50    0.30    --   70.00  78.00-122.44   50
 35  \w     92.00 176.00   0.50    1.20    --  107.74  77.00-180.00  168
 36  \w    115.00 174.00   0.50    1.20    --  107.74 125.00 -90.00  118
 37  \w    108.00 160.00   0.50    1.20    --  107.74  37.00 -90.00  104
 38  \w     98.00 156.00   0.50    1.20    --  107.74  37.00-120.00  116
 39  \w     86.00 153.00   0.50    1.20    --  107.74  77.00 -90.00  134
 40  \w    116.00 176.00   0.50    1.20    --  107.74 125.00 -60.00  120
 41  \w     97.00 144.00   0.50    1.20    --  107.74  37.00  60.00   94
 42  \w     95.00 174.00   0.50    1.20    --  107.74  57.00 150.00  158
 43  \w     95.00 172.00   0.50    1.20    --  107.74  57.00  90.00  154
 44  \w     80.00 113.00   0.50    1.20    --  107.74   0.00  60.00   66
 45  \w     85.00 178.00   0.50    1.20    --  107.74  77.00 120.00  186
 46  \w     87.00 166.00   0.50    1.20    --  107.74  77.00 -60.00  158
 47  \w     94.00 178.00   0.50    1.20    --  107.74  57.00-120.00  168
 48  \w     77.00 106.00   0.50    1.20    --  107.74 -99.00   0.00   58
 49  \w     49.00  75.00   0.50    1.20    --  107.74 -57.00 -30.00   52
 50  \w     47.00  74.00   0.50    1.20    --  107.74 -57.00  30.00   54
 51  \w     39.00  69.00   0.50    1.20    --  107.74 -99.00   0.00   60
 52  \w     39.00  65.00   0.50    1.20    --  107.74 -57.00  60.00   52
 53  \w     76.00 106.00   0.50    1.20    --  107.74 -99.00 120.00   60
 54  \w     48.00  74.00   0.50    1.20    --  107.74 -99.00 120.00   52
 55  \w     35.00 101.00   0.50    1.20    --  107.74 -99.00  60.00  132
 56  \w     35.00 105.00   0.50    1.20    --  107.74 -99.00 -60.00  140
 57  \w     69.00 105.00   0.50    1.20    --  107.74 -99.00-120.00   72
 58  \w     79.00 111.00   0.50    1.20    --  107.74-125.00-180.00   64
 59  \w     41.00  67.00   0.50    1.20    --  107.74 -57.00-150.00   52
 60  \w     37.00  68.00   0.50    1.20    --  107.74 -57.00 -90.00   62
 61  \w     35.00 106.00   0.50    1.20    --  107.74-103.00-130.00  142
 62  \w     35.00  62.00   0.50    1.20    --  107.74 -99.00-120.00   54
 63  \w     35.00  70.00   0.50    1.20    --  107.74-125.00-180.00   70
 64  \w     15.00  83.00   0.50    0.30    --   47.70-103.00-130.00  136
 65  \w     53.00  79.00   0.50    1.20    --  107.74   0.00  60.00   52
 66  \w     38.00  67.00   0.50    0.30    --   58.00  75.00-158.43   58
 67  \w    -66.00 -40.00   0.50    0.30    --  -62.00 -75.00 -19.81   52
 68  \w    -71.00 -45.00   0.50    0.30    --  -66.00 -72.00 -29.04   52
 69  \w    -72.00 -45.00   0.50    0.30    --  -66.00 -72.00 -84.53   54
 70  \w    -78.00 -53.00   0.50    1.20    --  -74.00 -73.00-127.54   50
 71  \w    -80.00 -54.00   0.50    1.20    --  -78.00 -79.00-100.38   52
 72  \w    -82.00 -55.00   0.50    1.20    --  -78.00 -76.00 -55.24   54
 73  \w    -80.00 -54.00   0.50    1.20    --  -74.00 -74.00 -12.86   52
 74  \w    -87.00 -61.00   0.50    1.20    --  -82.00 -72.00 -17.35   52
 75  \w    -90.00 -63.00   0.50    1.20    --  -86.25 -77.00 -60.00   54
 76  \w    -89.00 -63.00   0.50    1.20    --  -86.25 -77.00 -30.00   52
 77  \w    -94.00 -66.00   0.50    1.20    --  -86.25 -71.00   3.24   56
 78  \w    -97.00 -64.00   0.50    1.20    --  -86.00 -74.00 -20.28   66
 79  \w   -102.00 -63.00   0.50    1.20    --  -86.25 -78.00  58.73   78
 80  \w    -83.00 -57.00   0.50    1.20    --  -78.00 -78.00  96.51   52
 81  \w    -82.00 -56.00   0.50    1.20    --  -74.00 -66.00 132.57   52
 82  \w    -82.00 -56.00   0.50    1.20    --  -78.00 -75.00 133.57   52
 83  \w    -87.00 -62.00   0.50    1.20    --  -86.25 -80.00 162.46   50
 84  \w    -91.00 -63.00   0.50    1.20    --  -86.25 -77.00 120.00   56
 85  \w    -93.00 -66.00   0.50    1.20    --  -86.25 -74.00 102.79   54
 86  \w    -95.00 -64.00   0.50    1.20    --  -86.00 -77.00  70.90   62
 87  \w    -87.00 -36.00   0.50    0.30    --  -47.70 -19.00 150.00  102
 88  \w   -102.00 -66.00   0.50    1.20    --  -86.25 -70.00  77.44   72
 89  \w   -110.00 -67.00   0.50    1.20    --  -86.25 -77.00 150.00   86
 90  \w   -122.00 -96.00   0.50    0.30    --  -47.70 -19.00 150.00   52
 91  \w   -112.00 -63.00   0.50    1.20    --  -86.25 -77.00  43.39   98
 92  \w   -121.00 -38.00   0.50    0.30    --  -47.70 -19.00 -30.00  166
 93  \w    -92.00 -66.00   0.50    1.20    --  -86.25 -73.00-144.69   52
 94  \w    -82.00 -56.00   0.50    1.20    --  -78.00 -74.00-166.33   52
 95  \w    -96.00 -63.00   0.50    1.20    --  -86.25 -77.00-180.00   66
 96  \w    -91.00 -63.00   0.50    1.20    --  -86.25 -77.00-120.00   56
 97  \w    -97.00 -63.00   0.50    1.20    --  -86.25 -77.00 -90.00   68
 98  \w   -103.00 -67.00   0.50    1.20    --  -86.25 -67.00-174.92   72
 99  \w   -122.00 -44.00   0.50    0.30    --  -47.70 -19.00-120.00  156
100  \w    -81.00   7.00   0.50    0.30    --  -47.70 103.00 -28.00  176
101  \w    -81.00 -13.00   0.50    1.20    --  -86.25 103.00 -28.00  136
102  \w   -142.00-116.00   0.50    1.20    --  -86.25 -73.00-144.69   52
103  \w   -144.00-118.00   0.50    1.20    --  -86.25 -77.00-120.00   52
104  \w   -159.00 -84.00   0.50    1.20    --  -86.25-103.00-130.00  150
105  \w   -152.00-125.00   0.50    1.20    --  -86.25 -77.00 -60.00   54
106  \w   -145.00 -64.00   0.50    1.20    --  -86.25 -80.00  29.48  162
107  \w   -153.00-128.00   0.50    1.20    --  -86.25 -80.00 162.46   50
108  \w   -157.00-127.00   0.50    1.20    --  -86.25 -70.00  77.44   60
109  \w   -158.00-127.00   0.50    1.20    --  -86.25 -67.00-174.92   62
;
_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      0.0146588000
_diffrn_orient_matrix_UB_12      0.0158628000
_diffrn_orient_matrix_UB_13      -0.0921623000
_diffrn_orient_matrix_UB_21      0.0617148000
_diffrn_orient_matrix_UB_22      -0.0841978000
_diffrn_orient_matrix_UB_23      -0.0093853000
_diffrn_orient_matrix_UB_31      -0.2012271000
_diffrn_orient_matrix_UB_32      -0.0247219000
_diffrn_orient_matrix_UB_33      -0.0270566000
_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  0.0441
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            59089
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.373
_diffrn_reflns_theta_min         3.769
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.831
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.336
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_description       block
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.274
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.274
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0363
_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^)+8.6075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0845
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4222
_reflns_number_total             4295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra03383j2.cif
_cod_data_source_block           jv210503mo_01_cu_100k-gg
_cod_original_formula_sum        'C15.50 H22 B Cl F4 Mo O3 S2'
_cod_database_code               7246970
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C15 H21 S2 O3 Mo B F4'
_shelx_estimated_absorpt_t_max   0.843
_shelx_estimated_absorpt_t_min   0.271
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Others
 Sof(Cl2)=1-FVAR(1)
 Sof(Cl1)=FVAR(1)
 Fixed Sof: C16(0.5) H16a(0.5) H16b(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C9(H9a,H9b), C15(H15a,H15b), C13(H13a,H13b), C12(H12a,H12b),
 C14(H14a,H14b), C8(H8a,H8b), C16(H16a,H16b)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C7(H7)
3.c Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c)
;
_shelx_res_checksum              64393
_shelx_hkl_checksum              52257
_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 1.532
_oxdiff_exptl_absorpt_empirical_full_min 0.707