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_7248864
_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 H12 Mo N3 O5)'
_chemical_formula_sum            'C28 H24 Mo8 N6 O29'
_chemical_formula_weight         1676.05
_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   geom
_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                106.381(2)
_cell_angle_beta                 105.966(2)
_cell_angle_gamma                93.753(2)
_cell_formula_units_Z            1
_cell_length_a                   8.8403(2)
_cell_length_b                   9.1695(2)
_cell_length_c                   14.0494(3)
_cell_measurement_reflns_used    8579
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      77.2400
_cell_measurement_theta_min      3.4170
_cell_volume                     1037.78(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.973
_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    101.00 162.00   0.50    0.09    --  107.75  30.00   0.00  122
  2  \w     94.00 169.00   0.50    0.09    --  107.75  15.00  60.00  150
  3  \w     96.00 166.00   0.50    0.09    --  107.75  15.00 120.00  140
  4  \w     97.00 178.00   0.50    0.09    --  107.75  15.00 -30.00  162
  5  \w    106.00 131.00   0.50    0.09    --  107.75  15.00-180.00   50
  6  \w    141.00 177.00   0.50    0.09    --  107.75  15.00-180.00   72
  7  \w    100.00 176.00   0.50    0.09    --  107.75  30.00-120.00  152
  8  \w     73.00  98.00   0.50    0.09    --  107.75 -95.00  90.00   50
  9  \w     55.00 112.00   0.50    0.09    --  107.75-125.00  90.00  114
 10  \w     87.00 112.00   0.50    0.09    --  107.75-125.00  60.00   50
 11  \w     60.00  86.00   0.50    0.09    --  107.75-125.00  60.00   52
 12  \w     44.00 107.00   0.50    0.09    --  107.75-102.00  22.68  126
 13  \w     71.00 101.00   0.50    0.09    --  107.75 -96.00 137.00   60
 14  \w     -4.00  78.00   0.50    0.05    --   46.91 -96.00 137.00  164
 15  \w     46.00 101.00   0.50    0.09    --  107.75 -95.00 120.00  110
 16  \w     44.00 112.00   0.50    0.09    --  107.75-125.00 -60.00  136
 17  \w     73.00  99.00   0.50    0.09    --  107.75 -95.00-180.00   52
 18  \w     87.00 112.00   0.50    0.09    --  107.75-125.00-150.00   50
 19  \w     77.00 108.00   0.50    0.09    --  107.75-109.00 -66.79   62
 20  \w     60.00 104.00   0.50    0.09    --  107.75 -95.00 -60.00   88
 21  \w     36.00  91.00   0.50    0.09    --  107.75 -95.00 -30.00  110
 22  \w     38.00  69.00   0.50    0.09    --  107.75 -95.00  60.00   62
 23  \w     44.00  69.00   0.50    0.09    --  107.75 -95.00  90.00   50
 24  \w     77.00 103.00   0.50    0.09    --  107.75 -95.00  60.00   52
 25  \w     35.00  70.00   0.50    0.09    --  107.75 -95.00-180.00   70
 26  \w     62.00 104.00   0.50    0.09    --  107.75 -77.00 -60.00   84
 27  \w     42.00  73.00   0.50    0.09    --  107.75 -77.00-180.00   62
 28  \w     60.00  86.00   0.50    0.09    --  107.75 -77.00-150.00   52
 29  \w     36.00  71.00   0.50    0.09    --  107.75 -61.00-180.00   70
 30  \w     39.00  70.00   0.50    0.09    --  107.75 -77.00 -90.00   62
 31  \w    -19.00  25.00   0.50    0.05    --   46.91 -19.00-150.00   88
 32  \w     37.00  63.00   0.50    0.09    --  107.75 -77.00  60.00   52
 33  \w     46.00  87.00   0.50    0.09    --  107.75 -77.00  90.00   82
 34  \w     35.00  68.00   0.50    0.09    --  107.75 -61.00 120.00   66
 35  \w    117.00 165.00   0.50    0.09    --  107.75  96.00-114.00   96
 36  \w     98.00 123.00   0.50    0.09    --  107.75 125.00   0.00   50
 37  \w    115.00 140.00   0.50    0.09    --  107.75 125.00 -30.00   50
 38  \w    133.00 159.00   0.50    0.09    --  107.75 125.00   0.00   52
 39  \w    -43.00  -7.00   0.50    0.05    --  -46.91  38.00-150.00   72
 40  \w     -3.00  24.00   0.50    0.05    --  -46.91  38.00-150.00   54
 41  \w    -47.00 -14.00   0.50    0.09    --  -86.25  45.00 -90.00   66
 42  \w    -50.00 -14.00   0.50    0.09    --  -86.25  45.00  30.00   72
 43  \w    -50.00 -24.00   0.50    0.09    --  -86.25  45.00  90.00   52
 44  \w   -158.00-113.00   0.50    0.09    --  -86.25 -45.00 -30.00   90
 45  \w   -118.00 -78.00   0.50    0.05    --  -46.91-125.00 -60.00   80
 46  \w   -117.00 -73.00   0.50    0.05    --  -46.91-125.00-120.00   88
 47  \w   -118.00 -74.00   0.50    0.05    --  -46.91-125.00-150.00   88
 48  \w   -146.00-121.00   0.50    0.09    --  -86.25 -96.00 137.00   50
 49  \w    -53.00  25.00   0.50    0.05    --  -46.91  96.00-114.00  156
 50  \w    -71.00 -46.00   0.50    0.09    --  -86.25  96.00-114.00   50
;
_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      0.0042145000
_diffrn_orient_matrix_UB_12      -0.0083344000
_diffrn_orient_matrix_UB_13      -0.1102849000
_diffrn_orient_matrix_UB_21      0.0195869000
_diffrn_orient_matrix_UB_22      -0.1709326000
_diffrn_orient_matrix_UB_23      -0.0222202000
_diffrn_orient_matrix_UB_31      -0.1823794000
_diffrn_orient_matrix_UB_32      -0.0462017000
_diffrn_orient_matrix_UB_33      -0.0419713000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14341
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.001
_diffrn_reflns_theta_min         5.089
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.157
_exptl_absorpt_correction_T_max  0.04313
_exptl_absorpt_correction_T_min  0.00166
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'grayish red'
_exptl_crystal_colour_modifier   grayish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.682
_exptl_crystal_description       sphere
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.097
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.022
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         2.554
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.473
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0802
_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^)+(0.1417P)^2^+0.3354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1975
_refine_ls_wR_factor_ref         0.2002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4083
_reflns_number_total             4320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra03563a2.cif
_cod_data_source_block           3H
_cod_database_code               7248864
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo4 N3 O14 C13'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.665
_shelx_estimated_absorpt_t_min   0.245
_diffrn_oxdiff_digest_frames
;
01f90d87c4acf4f94707412155742f9f8f00065f6f2
;
_diffrn_oxdiff_digest_hkl
;
01225711ddc4f5e35f1d9ccd0135025aeb3cd5
;
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.068) H6(0.062) H12(0.073) H4(0.065) H3A(0.063) H13(0.067)
 H10(0.064) H14A(0.087) H14B(0.087) H14C(0.087) H11(0.076) H7(0.06)
 Fixed X: O9(0.5) H3(0.843001) H6(0.034671) H12(1.166743) H4(-0.099069)
 H3A(0.14621) H13(0.985487) H10(0.667946) H14A(-0.297274) H14B(-0.420762) H14C(-
 0.35138) H11(1.085859) H7(0.28176)
 Fixed Y: O9(0.5) H3(1.090816) H6(0.433785) H12(0.862807) H4(-0.030336) H3A(-
 0.050136) H13(0.631501) H10(0.878854) H14A(0.0213) H14B(0.14042)
 H14C(0.069816) H11(1.094625) H7(0.558578)
 Fixed Z: O9(1) H3(0.815363) H6(0.422509) H12(0.933974) H4(0.338511)
 H3A(0.44557) H13(0.837997) H10(0.719719) H14A(0.218156) H14B(0.228832)
 H14C(0.321029) H11(0.91723) H7(0.552819)
;
_shelx_res_checksum              11721
_shelx_hkl_checksum              5202
_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 2.035
_oxdiff_exptl_absorpt_empirical_full_min 0.401