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_7248860
_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), 2(C2 H3 N)'
_chemical_formula_sum            'C32 H30 Mo8 N8 O29'
_chemical_formula_weight         1758.16
_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             2022-04-29
_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                73.422(2)
_cell_angle_beta                 72.752(2)
_cell_angle_gamma                66.204(2)
_cell_formula_units_Z            1
_cell_length_a                   10.02310(10)
_cell_length_b                   10.7273(3)
_cell_length_c                   12.9277(3)
_cell_measurement_reflns_used    11444
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      77.3170
_cell_measurement_theta_min      3.6510
_cell_volume                     1192.60(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.980
_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    103.00 132.00   0.50    0.33    --  107.75  77.00 -60.00   58
  2  \w    137.00 162.00   0.50    0.33    --  107.75  77.00 -60.00   50
  3  \w    106.00 174.00   0.50    0.33    --  107.75  45.00-150.00  136
  4  \w     98.00 176.00   0.50    0.33    --  107.75  45.00 -60.00  156
  5  \w    105.00 146.00   0.50    0.33    --  107.75  15.00-150.00   82
  6  \w    110.00 178.00   0.50    0.33    --  107.75  45.00  30.00  136
  7  \w    120.00 174.00   0.50    0.33    --  107.75  45.00  60.00  108
  8  \w     95.00 123.00   0.50    0.33    --  107.75  30.00 120.00   56
  9  \w    128.00 154.00   0.50    0.33    --  107.75  30.00 120.00   52
 10  \w    -24.00  26.00   0.50    0.08    --  -47.03  19.00-120.00  100
 11  \w     -8.00  27.00   0.50    0.08    --  -47.03  19.00 -90.00   70
 12  \w    -44.00 -14.00   0.50    0.33    --  -86.25  45.00   0.00   60
 13  \w    -17.00   8.00   0.50    0.08    --  -47.03  19.00  30.00   50
 14  \w    -25.00  28.00   0.50    0.08    --  -47.03  19.00 150.00  106
 15  \w    100.00 154.00   0.50    0.33    --  107.75 121.00 128.00  108
 16  \w    136.00 161.00   0.50    0.33    --  107.75 125.00  60.00   50
 17  \w     95.00 121.00   0.50    0.33    --  107.75 125.00  60.00   52
 18  \w     94.00 119.00   0.50    0.33    --  107.75 155.00 -73.00   50
 19  \w     95.00 174.00   0.50    0.33    --  107.75 125.00 -30.00  158
 20  \w    -21.00  25.00   0.50    0.08    --   47.03 -19.00   0.00   92
 21  \w     37.00  89.00   0.50    0.33    --  107.75 -77.00 150.00  104
 22  \w     61.00  86.00   0.50    0.33    --  107.75 -77.00  90.00   50
 23  \w     37.00  64.00   0.50    0.33    --  107.75 -61.00 120.00   54
 24  \w     55.00 105.00   0.50    0.33    --  107.75 -77.00  30.00  100
 25  \w     35.00  71.00   0.50    0.33    --  107.75 -61.00  30.00   72
 26  \w     40.00  67.00   0.50    0.33    --  107.75 -61.00   0.00   54
 27  \w     37.00  69.00   0.50    0.33    --  107.75 -61.00 -60.00   64
 28  \w     35.00  64.00   0.50    0.33    --  107.75 -61.00-120.00   58
 29  \w     39.00  64.00   0.50    0.33    --  107.75 -61.00-150.00   50
 30  \w     71.00  96.00   0.50    0.33    --  107.75 -77.00 -90.00   50
 31  \w     37.00  71.00   0.50    0.33    --  107.75 -61.00  60.00   68
 32  \w     44.00  69.00   0.50    0.33    --  107.75 -61.00  90.00   50
 33  \w     76.00 102.00   0.50    0.33    --  107.75 -95.00 -60.00   52
 34  \w     81.00 107.00   0.50    0.33    --  107.75-125.00-120.00   52
 35  \w     74.00 133.00   0.50    0.33    --  107.75-155.00-112.00  118
 36  \w     58.00 113.00   0.50    0.08    --   47.03-155.00-112.00  110
 37  \w     64.00 112.00   0.50    0.33    --  107.75-125.00 -90.00   96
 38  \w     40.00 111.00   0.50    0.33    --  107.75-125.00 -60.00  142
 39  \w     37.00 112.00   0.50    0.33    --  107.75-125.00  30.00  150
 40  \w     83.00 109.00   0.50    0.33    --  107.75-125.00  90.00   52
 41  \w     80.00 108.00   0.50    0.33    --  107.75-125.00 150.00   56
 42  \w     86.00 111.00   0.50    0.33    --  107.75-125.00 120.00   50
 43  \w     35.00  67.00   0.50    0.33    --  107.75-125.00 150.00   64
 44  \w     40.00  93.00   0.50    0.08    --   47.03-121.00  45.00  106
 45  \w     72.00 109.00   0.50    0.33    --  107.75-121.00  45.00   74
 46  \w     58.00  84.00   0.50    0.33    --  107.75 -95.00  60.00   52
 47  \w     38.00  69.00   0.50    0.33    --  107.75 -95.00 -60.00   62
 48  \w     38.00  68.00   0.50    0.33    --  107.75-125.00-180.00   60
 49  \w     79.00 109.00   0.50    0.33    --  107.75-125.00-180.00   60
 50  \w   -125.00 -88.00   0.50    0.33    --  -86.25 -30.00 -90.00   74
 51  \w   -123.00 -98.00   0.50    0.33    --  -86.25-155.00-112.00   50
 52  \w    -95.00 -53.00   0.50    0.08    --  -47.03-155.00-112.00   84
 53  \w   -114.00 -79.00   0.50    0.33    --  -86.25-121.00  45.00   70
 54  \w   -107.00 -82.00   0.50    0.08    --  -47.03-125.00  60.00   50
 55  \w    -40.00 -14.00   0.50    0.08    --  -47.03 121.00 128.00   52
 56  \w    -56.00 -29.00   0.50    0.33    --  -86.25 121.00 128.00   54
 57  \w    -81.00 -55.00   0.50    0.08    --  -47.03 155.00 -73.00   52
 58  \w    -92.00 -67.00   0.50    0.33    --  -86.25 155.00 -73.00   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      -0.0389136000
_diffrn_orient_matrix_UB_12      0.1523517000
_diffrn_orient_matrix_UB_13      0.0063754000
_diffrn_orient_matrix_UB_21      -0.0146922000
_diffrn_orient_matrix_UB_22      -0.0411725000
_diffrn_orient_matrix_UB_23      0.1260953000
_diffrn_orient_matrix_UB_31      0.1665804000
_diffrn_orient_matrix_UB_32      -0.0254426000
_diffrn_orient_matrix_UB_33      -0.0144812000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17780
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.711
_diffrn_reflns_theta_min         3.646
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.600
_exptl_absorpt_correction_T_max  0.696
_exptl_absorpt_correction_T_min  0.149
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.448
_exptl_crystal_description       irregular
_exptl_crystal_F_000             846
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.475
_refine_diff_density_min         -1.265
_refine_diff_density_rms         0.200
_refine_ls_extinction_coef       0.00047(8)
_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   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0604P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4572
_reflns_number_total             4996
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra03563a2.cif
_cod_data_source_block           3H-2CH3CN
_cod_database_code               7248860
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo8 O25 C30 N8'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.611
_shelx_estimated_absorpt_t_min   0.158
_diffrn_oxdiff_digest_frames
;
0140d9eb0e04fff2879d2bbf85e9a92cb80439634f0
;
_diffrn_oxdiff_digest_hkl
;
013db9e7c0544c078e89abe526e7f38d8c5bc3
;
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.022) H7(0.021) H10(0.022) H4(0.027) H6(0.025) H3A(0.026)
 H14A(0.036) H14B(0.036) H14C(0.036) H13(0.024) H11(0.026) H12(0.027)
 H16A(0.092) H16B(0.092) H16C(0.092)
 Fixed X: O11(0) H3(0.506666) H7(0.743632) H10(0.543561) H4(0.821504)
 H6(0.836937) H3A(0.702669) H14A(0.853293) H14B(0.993632) H14C(1.010493)
 H13(0.65012) H11(0.537928) H12(0.612386) H16A(0.134989) H16B(0.182689)
 H16C(0.087366)
 Fixed Y: O11(0.5) H3(0.252803) H7(-0.028288) H10(0.328639) H4(0.210967) H6(-
 0.085421) H3A(0.383256) H14A(0.023577) H14B(-0.118002) H14C(0.021655) H13(-
 0.066861) H11(0.032199) H12(-0.134297) H16A(0.462677) H16B(0.407933)
 H16C(0.33984)
 Fixed Z: O11(0.5) H3(0.776525) H7(0.229842) H10(0.594342) H4(-0.225097)
 H6(0.052113) H3A(-0.117414) H14A(-0.299413) H14B(-0.297794) H14C(-0.291541)
 H13(0.56187) H11(0.862593) H12(0.753399) H16A(1.013769) H16B(1.130884)
 H16C(1.100024)
;
_shelx_res_checksum              10659
_shelx_hkl_checksum              22442
_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 1.876
_oxdiff_exptl_absorpt_empirical_full_min 0.519