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_7246967
_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         'C11 H11 Mo N2 O2, C F3 O3 S'
_chemical_formula_sum            'C12 H11 F3 Mo N2 O5 S'
_chemical_formula_weight         448.23
_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     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                 90.3980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.89540(10)
_cell_length_b                   10.32310(10)
_cell_length_c                   14.51370(10)
_cell_measurement_reflns_used    37750
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.0020
_cell_measurement_theta_min      4.0380
_cell_volume                     1632.38(2)
_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     31.00 120.00   0.50    0.11    --   47.70  63.00-147.33  178
  2  \w     31.00 120.00   0.50    0.11    --   47.70  62.00-112.38  178
  3  \w     32.00 120.00   0.50    0.11    --   47.70  59.00 -24.65  176
  4  \w     33.00 120.00   0.50    0.11    --   47.70  57.00   0.00  174
  5  \w     33.00 120.00   0.50    0.11    --   47.70  57.00  30.00  174
  6  \w     33.00 120.00   0.50    0.11    --   47.70  57.00  60.00  174
  7  \w     33.00 120.00   0.50    0.11    --   47.70  57.00  90.00  174
  8  \w     33.00 120.00   0.50    0.11    --   47.70  57.00 120.00  174
  9  \w     33.00 120.00   0.50    0.11    --   47.70  57.00 150.00  174
 10  \w     31.00 120.00   0.50    0.11    --   47.70  63.00 176.22  178
 11  \w    -86.00 -13.00   0.50    0.11    --  -47.70 125.00  30.00  146
 12  \w    -83.00 -58.00   0.50    0.43    --  -86.25  87.00  26.00   50
 13  \w    -75.00  25.00   0.50    0.11    --  -47.70  87.00  26.00  200
 14  \w    -42.00  26.00   0.50    0.11    --  -47.70  37.00 -30.00  136
 15  \w    102.00 176.00   0.50    0.43    --  107.74  77.00  90.00  148
 16  \w     96.00 172.00   0.50    0.43    --  107.74  57.00  60.00  152
 17  \w    103.00 174.00   0.50    0.43    --  107.74  37.00   0.00  142
 18  \w    140.00 177.00   0.50    0.43    --  107.74  37.00 -60.00   74
 19  \w    135.00 178.00   0.50    0.43    --  107.74  57.00-140.71   86
 20  \w     93.00 129.00   0.50    0.43    --  107.74  57.00-140.71   72
 21  \w     96.00 177.00   0.50    0.43    --  107.74  37.00-180.00  162
 22  \w    134.00 178.00   0.50    0.43    --  107.74  19.00 -90.00   88
 23  \w     99.00 136.00   0.50    0.43    --  107.74  37.00 -60.00   74
 24  \w    133.00 176.00   0.50    0.43    --  107.74  37.00 120.00   86
 25  \w    101.00 178.00   0.50    0.43    --  107.74  87.00  26.00  154
 26  \w     76.00 104.00   0.50    0.43    --  107.74 -77.00 120.00   56
 27  \w     41.00  73.00   0.50    0.43    --  107.74 -77.00 120.00   64
 28  \w     36.00  66.00   0.50    0.43    --  107.74 -57.00 150.00   60
 29  \w     35.00  81.00   0.50    0.43    --  107.74 -77.00   0.00   92
 30  \w     36.00  64.00   0.50    0.43    --  107.74 -57.00   0.00   56
 31  \w     37.00  66.00   0.50    0.43    --  107.74 -57.00 120.00   58
 32  \w     39.00  70.00   0.50    0.43    --  107.74 -77.00 -30.00   62
 33  \w     37.00  65.00   0.50    0.43    --  107.74 -57.00 -90.00   56
 34  \w     35.00  61.00   0.50    0.43    --  107.74 -57.00-120.00   52
 35  \w     40.00  65.00   0.50    0.43    --  107.74 -57.00-180.00   50
 36  \w     35.00 135.00   0.50    0.43    --  107.74 -87.00 -90.00  200
 37  \w     82.00 110.00   0.50    0.43    --  107.74-120.00-179.54   56
 38  \w     43.00 124.00   0.50    0.43    --  107.74-141.00 -90.07  162
 39  \w     70.00 110.00   0.50    0.43    --  107.74-125.00  30.00   80
 40  \w     36.00  61.00   0.50    0.43    --  107.74-125.00  30.00   50
 41  \w     40.00 117.00   0.50    0.43    --  107.74-134.00 102.33  154
 42  \w     37.00 106.00   0.50    0.43    --  107.74 -99.00  90.00  138
 43  \w     38.00  75.00   0.50    0.43    --  107.74 -99.00 120.00   74
 44  \w     38.00 103.00   0.50    0.43    --  107.74 -99.00 -90.00  130
 45  \w    -21.00  75.00   0.50    0.11    --   47.70 -87.00 -90.00  192
 46  \w   -119.00 -33.00   0.50    0.11    --  -47.70 -57.00-150.00  172
 47  \w   -119.00 -33.00   0.50    0.11    --  -47.70 -57.00-120.00  172
 48  \w   -120.00 -34.00   0.50    0.11    --  -47.70 -43.00-100.87  172
 49  \w   -121.00 -35.00   0.50    0.11    --  -47.70 -37.00 -30.00  172
 50  \w   -121.00 -35.00   0.50    0.11    --  -47.70 -37.00 120.00  172
 51  \w    -97.00 -71.00   0.50    0.43    --  -86.25 -64.00 116.41   52
 52  \w   -159.00 -69.00   0.50    0.43    --  -86.25 -63.00 160.29  180
 53  \w   -159.00 -69.00   0.50    0.43    --  -86.25 -63.00  16.68  180
 54  \w    -98.00 -71.00   0.50    0.43    --  -86.25 -63.00  47.32   54
 55  \w   -159.00 -69.00   0.50    0.43    --  -86.25 -62.00  59.99  180
 56  \w   -159.00 -69.00   0.50    0.43    --  -86.25 -63.00 -21.67  180
 57  \w    -95.00 -69.00   0.50    0.43    --  -86.25 -62.00 -30.91   52
 58  \w   -159.00 -69.00   0.50    0.43    --  -86.25 -63.00 -53.34  180
 59  \w   -157.00-119.00   0.50    0.43    --  -86.25 -62.00 -30.91   76
 60  \w    -96.00 -70.00   0.50    0.43    --  -86.25 -61.00 -47.70   52
 61  \w   -159.00 -70.00   0.50    0.43    --  -86.25 -61.00  20.96  178
 62  \w   -159.00 -70.00   0.50    0.43    --  -86.25 -61.00 -86.58  178
 63  \w    -94.00 -69.00   0.50    0.43    --  -86.25 -63.00-165.70   50
 64  \w    -96.00 -70.00   0.50    0.43    --  -86.25 -61.00-125.15   52
 65  \w   -158.00 -70.00   0.50    0.43    --  -86.25 -60.00  91.48  176
 66  \w   -158.00 -70.00   0.50    0.43    --  -86.25 -60.00 143.63  176
 67  \w   -158.00 -70.00   0.50    0.43    --  -86.25 -60.00 137.13  176
 68  \w   -158.00 -70.00   0.50    0.43    --  -86.25 -60.00  77.63  176
 69  \w   -159.00 -71.00   0.50    0.43    --  -86.25 -57.00  30.00  176
 70  \w   -159.00 -71.00   0.50    0.43    --  -86.25 -57.00  -6.00  176
 71  \w   -155.00 -70.00   0.50    0.43    --  -86.25 -60.00 -69.11  170
 72  \w   -158.00 -70.00   0.50    0.43    --  -86.25 -60.00-149.06  176
 73  \w    -99.00 -70.00   0.50    0.43    --  -86.25 -59.00-116.27   58
 74  \w   -104.00 -71.00   0.50    0.43    --  -86.25 -56.00-113.18   66
 75  \w    -96.00 -71.00   0.50    0.43    --  -86.25 -57.00-143.94   50
 76  \w   -131.00-105.00   0.50    0.43    --  -86.25 -57.00-143.94   52
 77  \w    -97.00 -71.00   0.50    0.43    --  -86.25 -57.00 120.00   52
 78  \w   -159.00 -71.00   0.50    0.43    --  -86.25 -56.00 163.12  176
 79  \w   -159.00 -71.00   0.50    0.43    --  -86.25 -57.00 -16.53  176
 80  \w   -159.00 -79.00   0.50    0.43    --  -86.25 -87.00 -90.00  160
;
_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      -0.0561230000
_diffrn_orient_matrix_UB_12      0.0763339000
_diffrn_orient_matrix_UB_13      -0.0812007000
_diffrn_orient_matrix_UB_21      -0.1240977000
_diffrn_orient_matrix_UB_22      0.0046654000
_diffrn_orient_matrix_UB_23      0.0501160000
_diffrn_orient_matrix_UB_31      0.0378768000
_diffrn_orient_matrix_UB_32      0.1281807000
_diffrn_orient_matrix_UB_33      0.0465093000
_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  0.0459
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            54376
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.586
_diffrn_reflns_theta_max         66.586
_diffrn_reflns_theta_min         4.058
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.335
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.548
_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    1.824
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0165
_refine_ls_R_factor_gt           0.0157
_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^)+(0.0197P)^2^+0.8896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0399
_refine_ls_wR_factor_ref         0.0403
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2761
_reflns_number_total             2882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra03383j2.cif
_cod_data_source_block           jv201111mo_10_cu_100k-gg
_cod_database_code               7246967
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C12 H11 F3 Mo N2 O5 S '
_shelx_estimated_absorpt_t_max   0.788
_shelx_estimated_absorpt_t_min   0.489
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C5(H5), C3(H3), C6(H6), C4(H4)
2.b Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C11(H11a,H11b,H11c)
;
_shelx_res_checksum              40759
_shelx_hkl_checksum              27390
_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 1.583
_oxdiff_exptl_absorpt_empirical_full_min 0.606