Impact of POM's coordination mode and Mo-hybrid constituents on the binding, stability, and catalytic properties of hybrid (pre)catalysts
Pisk, Jana; Vrdoljak, Višnja; Mandarić, Mirna; Hrenar, Tomica; Agustin, Dominique; Rubčić, Mirta; RSC Advances 14 (2024) 19029–19040; doi:10.1039/D4RA03563A

data_7248863
_publ_section_title
;
 Impact of POM's coordination mode and Mo-hybrid constituents on the
 binding, stability, and catalytic properties of hybrid (pre)catalysts
;
_journal_issue                   27
_journal_name_full               'RSC Advances'
_journal_page_first              19029
_journal_page_last               19040
_journal_paper_doi               10.1039/D4RA03563A
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'Mo6 O19, 2(C14 H14 Mo N3 O6), 2(C3 H6 O)'
_chemical_formula_sum            'C34 H40 Mo8 N6 O33'
_chemical_formula_weight         1828.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-02-27 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                106.660(5)
_cell_angle_beta                 106.352(6)
_cell_angle_gamma                99.224(5)
_cell_formula_units_Z            1
_cell_length_a                   10.6083(8)
_cell_length_b                   10.7813(6)
_cell_length_c                   12.8485(6)
_cell_measurement_reflns_used    8960
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      78.9620
_cell_measurement_theta_min      3.8490
_cell_volume                     1303.62(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_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    105.00 139.00   0.50    0.05    --  113.25  30.00  60.00   68
  2  \w    118.00 174.00   0.50    0.05    --  113.25  45.00 -30.00  112
  3  \w    120.00 178.00   0.50    0.05    --  113.25  45.00 -90.00  116
  4  \w    149.00 175.00   0.50    0.05    --  113.25  61.00-120.00   52
  5  \w     98.00 138.00   0.50    0.05    --  113.25  61.00-120.00   80
  6  \w    100.00 126.00   0.50    0.05    --  113.25  15.00-150.00   52
  7  \w    131.00 178.00   0.50    0.05    --  113.25  15.00-150.00   94
  8  \w    137.00 163.00   0.50    0.05    --  113.25  30.00-120.00   52
  9  \w    127.00 177.00   0.50    0.05    --  113.25   0.00  90.00  100
 10  \w     54.00 118.00   0.50    0.05    --  113.25   0.00  90.00  128
 11  \w     77.00 103.00   0.50    0.05    --  113.25 -95.00 -30.00   52
 12  \w     80.00 107.00   0.50    0.05    --  113.25-125.00   0.00   54
 13  \w     92.00 133.00   0.50    0.05    --  113.25-156.00  14.19   82
 14  \w     85.00 110.00   0.50    0.05    --  113.25-125.00 -90.00   50
 15  \w     56.00  84.00   0.50    0.05    --  113.25-156.00  14.19   56
 16  \w     63.00 111.00   0.50    0.05    --  113.25-125.00 -60.00   96
 17  \w     46.00  78.00   0.50    0.05    --  113.25-125.00 -90.00   64
 18  \w     46.00  74.00   0.50    0.05    --  113.25-125.00   0.00   56
 19  \w     48.00  77.00   0.50    0.05    --  113.25-125.00  60.00   58
 20  \w     81.00 106.00   0.50    0.05    --  113.25-125.00 120.00   50
 21  \w     52.00 110.00   0.50    0.05    --  113.25-125.00 150.00  116
 22  \w     47.00  75.00   0.50    0.05    --  113.25-125.00 120.00   56
 23  \w     86.00 111.00   0.50    0.05    --  113.25-125.00  60.00   50
 24  \w     84.00 109.00   0.50    0.05    --  113.25-115.00  79.31   50
 25  \w     42.00  74.00   0.50    0.05    --  113.25-115.00  79.31   64
 26  \w     83.00 108.00   0.50    0.05    --  113.25-106.00  39.46   50
 27  \w     82.00 111.00   0.50    0.05    --  113.25-125.00-180.00   58
 28  \w     84.00 109.00   0.50    0.05    --  113.25-113.00-176.00   50
 29  \w     51.00  77.00   0.50    0.05    --  113.25-113.00-176.00   52
 30  \w     26.00  67.00   0.50    0.05    --   48.02-113.00-176.00   82
 31  \w     43.00  97.00   0.50    0.05    --  113.25 -95.00   0.00  108
 32  \w     57.00 106.00   0.50    0.05    --  113.25 -95.00 150.00   98
 33  \w     42.00  77.00   0.50    0.05    --  113.25 -95.00 -60.00   70
 34  \w     66.00  92.00   0.50    0.05    --  113.25 -95.00-120.00   52
 35  \w     42.00  71.00   0.50    0.05    --  113.25 -61.00-180.00   58
 36  \w     80.00 105.00   0.50    0.05    --  113.25 -77.00-180.00   50
 37  \w     80.00 105.00   0.50    0.05    --  113.25 -77.00  30.00   50
 38  \w     72.00 104.00   0.50    0.05    --  113.25 -77.00 150.00   64
 39  \w     46.00  71.00   0.50    0.05    --  113.25 -61.00 150.00   50
 40  \w     44.00  70.00   0.50    0.05    --  113.25 -77.00 120.00   52
 41  \w     42.00  70.00   0.50    0.05    --  113.25 -61.00  30.00   56
 42  \w     42.00  68.00   0.50    0.05    --  113.25 -61.00  60.00   52
 43  \w     46.00  71.00   0.50    0.05    --  113.25 -61.00 -30.00   50
 44  \w     42.00  67.00   0.50    0.05    --  113.25 -61.00 -60.00   50
 45  \w     45.00  71.00   0.50    0.05    --  113.25 -61.00-120.00   52
 46  \w    112.00 161.00   0.50    0.05    --  113.25 113.00 -85.00   98
 47  \w    -63.00  23.00   0.50    0.05    --  -48.02  57.00-150.00  172
 48  \w    -47.00 -19.00   0.50    0.05    --  -91.75 113.00 -85.00   56
 49  \w    -33.00  -7.00   0.50    0.05    --  -48.02 113.00 -85.00   52
 50  \w    -82.00 -43.00   0.50    0.05    --  -48.02 113.00 -85.00   78
 51  \w    -56.00 -12.00   0.50    0.05    --  -48.02  57.00 -60.00   88
 52  \w     -8.00  20.00   0.50    0.05    --  -48.02  57.00 -60.00   56
 53  \w    -49.00 -24.00   0.50    0.05    --  -91.75  45.00   0.00   50
 54  \w    -51.00 -26.00   0.50    0.05    --  -91.75  45.00 150.00   50
 55  \w    -48.00 -20.00   0.50    0.05    --  -91.75  45.00-150.00   56
 56  \w   -161.00 -79.00   0.50    0.05    --  -91.75 -30.00-120.00  164
 57  \w    -63.00 -27.00   0.50    0.05    --  -48.02 -77.00  90.00   72
 58  \w   -119.00 -91.00   0.50    0.05    --  -48.02 -77.00  90.00   56
 59  \w   -114.00 -84.00   0.50    0.05    --  -48.02-125.00   0.00   60
 60  \w   -120.00 -95.00   0.50    0.05    --  -48.02-125.00 -30.00   50
 61  \w   -101.00 -73.00   0.50    0.05    --  -48.02-125.00-150.00   56
 62  \w   -111.00 -85.00   0.50    0.05    --  -91.75-113.00-176.00   52
;
_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      -0.1431202000
_diffrn_orient_matrix_UB_12      -0.0814471000
_diffrn_orient_matrix_UB_13      -0.0864133000
_diffrn_orient_matrix_UB_21      0.0386801000
_diffrn_orient_matrix_UB_22      0.0315457000
_diffrn_orient_matrix_UB_23      -0.0983194000
_diffrn_orient_matrix_UB_31      0.0511467000
_diffrn_orient_matrix_UB_32      -0.1275135000
_diffrn_orient_matrix_UB_33      -0.0257796000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0926
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17776
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.310
_diffrn_reflns_theta_min         3.828
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.182
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.329
_exptl_crystal_description       plate
_exptl_crystal_F_000             886
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.063
_refine_diff_density_min         -2.045
_refine_diff_density_rms         0.303
_refine_ls_extinction_coef       0.0016(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5531
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0634
_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^)+(0.1315P)^2^+0.0170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1747
_refine_ls_wR_factor_ref         0.1820
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4949
_reflns_number_total             5531
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra03563a2.cif
_cod_data_source_block           3Hw-2CH3COCH3
_cod_original_cell_volume        1303.61(15)
_cod_database_code               7248863
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo C H N O'
_shelx_estimated_absorpt_t_max   0.498
_shelx_estimated_absorpt_t_min   0.247
_diffrn_oxdiff_digest_frames
;
01a044f0fd73342bcc4865e384e96ff298042784e87
;
_diffrn_oxdiff_digest_hkl
;
01d69c7dd92c417b09bc5ce8fd313b25ff3252
;
_reflns_odcompleteness_completeness 99.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.049) H6B(0.049) H6(0.029) H7(0.028) H12(0.05) H3(0.035)
 H14A(0.049) H14B(0.049) H14C(0.049) H4(0.034) H13(0.036) H3A(0.07) H10(0.045)
 H11(0.067) H15A(0.08) H15B(0.08) H15C(0.08) H17A(0.103) H17B(0.103) H17C(0.103)
 Fixed X: O11(1) H6A(0.64096) H6B(0.760188) H6(0.318353) H7(0.404503)
 H12(0.844415) H3(0.706732) H14A(0.138381) H14B(0.11845) H14C(0.197132)
 H4(0.528455) H13(0.841973) H3A(0.481824) H10(0.475214) H11(0.654803)
 H15A(0.28384) H15B(0.272355) H15C(0.403856) H17A(0.043088) H17B(0.053905)
 H17C(0.066837)
 Fixed Y: O11(1) H6A(0.671281) H6B(0.771894) H6(0.454304) H7(0.397213)
 H12(0.282406) H3(0.80666) H14A(0.514244) H14B(0.490669) H14C(0.403175)
 H4(0.763909) H13(0.404144) H3A(0.050493) H10(0.162773) H11(0.10393) H15A(-
 0.256877) H15B(-0.113152) H15C(-0.12553) H17A(-0.127116) H17B(-0.250087) H17C(-
 0.260289)
 Fixed Z: O11(0.5) H6A(0.566791) H6B(0.62066) H6(0.79826) H7(0.645255)
 H12(0.229776) H3(1.030918) H14A(0.862586) H14B(0.97501) H14C(0.906056)
 H4(1.099409) H13(0.406384) H3A(0.165894) H10(0.342105) H11(0.101397)
 H15A(0.21536) H15B(0.286389) H15C(0.250595) H17A(0.058251) H17B(0.103459)
 H17C(-0.019672)
;
_shelx_res_checksum              90974
_shelx_hkl_checksum              39556
_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 3.752
_oxdiff_exptl_absorpt_empirical_full_min 0.476