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_7248858
_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             2022-04-29
_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                74.262(5)
_cell_angle_beta                 72.168(5)
_cell_angle_gamma                88.125(4)
_cell_formula_units_Z            1
_cell_length_a                   8.8506(5)
_cell_length_b                   9.2538(5)
_cell_length_c                   14.0175(8)
_cell_measurement_reflns_used    8984
_cell_measurement_temperature    170
_cell_measurement_theta_max      79.3820
_cell_measurement_theta_min      3.3430
_cell_volume                     1050.34(11)
_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_temperature      170
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.972
_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     97.00 141.00   0.50    0.12    --  113.25  61.00   0.00   88
  2  \w    147.00 173.00   0.50    0.12    --  113.25  61.00   0.00   52
  3  \w    102.00 154.00   0.50    0.12    --  113.25  56.00-103.00  104
  4  \w     99.00 171.00   0.50    0.12    --  113.25  61.00-180.00  144
  5  \w     87.00 119.00   0.50    0.05    --   47.77  56.00-103.00   64
  6  \w    108.00 169.00   0.50    0.12    --  113.25  45.00 -30.00  122
  7  \w    143.00 169.00   0.50    0.12    --  113.25  45.00  60.00   52
  8  \w    153.00 178.00   0.50    0.12    --  113.25  15.00 120.00   50
  9  \w    101.00 149.00   0.50    0.12    --  113.25  15.00 120.00   96
 10  \w    102.00 174.00   0.50    0.12    --  113.25  45.00 150.00  144
 11  \w    107.00 157.00   0.50    0.12    --  113.25 125.00 -90.00  100
 12  \w    145.00 178.00   0.50    0.12    --  113.25 125.00-120.00   66
 13  \w     96.00 169.00   0.50    0.12    --  113.25 125.00-180.00  146
 14  \w     95.00 134.00   0.50    0.12    --  113.25 125.00-120.00   78
 15  \w    137.00 163.00   0.50    0.12    --  113.25 125.00 150.00   52
 16  \w    -71.00 -22.00   0.50    0.12    --  -91.75  61.00  90.00   98
 17  \w    -51.00 -25.00   0.50    0.12    --  -91.75  45.00   0.00   52
 18  \w    -11.00  24.00   0.50    0.05    --  -47.77  56.00-103.00   70
 19  \w    -61.00 -14.00   0.50    0.05    --  -47.77  56.00-103.00   94
 20  \w    -53.00 -21.00   0.50    0.12    --  -91.75  56.00-103.00   64
 21  \w   -119.00 -34.00   0.50    0.05    --  -47.77 -56.00 114.00  170
 22  \w   -160.00-116.00   0.50    0.12    --  -91.75 -56.00 114.00   88
 23  \w   -111.00 -73.00   0.50    0.05    --  -47.77-125.00  60.00   76
 24  \w    -26.00  15.00   0.50    0.05    --   47.77 -19.00  30.00   82
 25  \w    -23.00   3.00   0.50    0.05    --   47.77 -56.00 114.00   52
 26  \w    -21.00  26.00   0.50    0.05    --   47.77 -19.00 120.00   94
 27  \w     28.00  53.00   0.50    0.05    --   47.77 -56.00 114.00   50
 28  \w     56.00  82.00   0.50    0.12    --  113.25-136.00  44.35   52
 29  \w     95.00 120.00   0.50    0.12    --  113.25-136.00  44.35   50
 30  \w     51.00 111.00   0.50    0.12    --  113.25-125.00  60.00  120
 31  \w     81.00 110.00   0.50    0.12    --  113.25-125.00  90.00   58
 32  \w     45.00 110.00   0.50    0.12    --  113.25-125.00   0.00  130
 33  \w     42.00  67.00   0.50    0.12    --  113.25-125.00 -30.00   50
 34  \w     84.00 110.00   0.50    0.12    --  113.25-125.00 -30.00   52
 35  \w     86.00 111.00   0.50    0.12    --  113.25-125.00 -90.00   50
 36  \w     52.00 107.00   0.50    0.12    --  113.25-125.00-150.00  110
 37  \w     51.00 109.00   0.50    0.12    --  113.25-125.00-180.00  116
 38  \w     62.00  88.00   0.50    0.05    --   47.77-125.00-180.00   52
 39  \w     79.00 105.00   0.50    0.12    --  113.25 -95.00-180.00   52
 40  \w     45.00  93.00   0.50    0.12    --  113.25 -95.00-150.00   96
 41  \w     35.00  94.00   0.50    0.05    --   47.77-125.00 -30.00  118
 42  \w     45.00 107.00   0.50    0.12    --  113.25-104.00 110.54  124
 43  \w     63.00  89.00   0.50    0.12    --  113.25-108.00  -0.57   52
 44  \w     64.00  94.00   0.50    0.12    --  113.25 -95.00 -90.00   60
 45  \w     43.00  90.00   0.50    0.12    --  113.25 -77.00-150.00   94
 46  \w     43.00  68.00   0.50    0.12    --  113.25 -61.00-150.00   50
 47  \w     42.00  91.00   0.50    0.12    --  113.25 -77.00 -90.00   98
 48  \w     43.00  68.00   0.50    0.12    --  113.25 -61.00 -90.00   50
 49  \w     50.00  85.00   0.50    0.12    --  113.25 -77.00  60.00   70
 50  \w     42.00  67.00   0.50    0.12    --  113.25 -61.00  90.00   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      -0.0856027000
_diffrn_orient_matrix_UB_12      0.0723405000
_diffrn_orient_matrix_UB_13      -0.0804163000
_diffrn_orient_matrix_UB_21      0.0636886000
_diffrn_orient_matrix_UB_22      0.1567916000
_diffrn_orient_matrix_UB_23      -0.0071239000
_diffrn_orient_matrix_UB_31      0.1488294000
_diffrn_orient_matrix_UB_32      -0.0137772000
_diffrn_orient_matrix_UB_33      -0.0888688000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_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            13693
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.012
_diffrn_reflns_theta_min         3.444
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.916
_exptl_absorpt_correction_T_max  0.04478
_exptl_absorpt_correction_T_min  0.00174
_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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.650
_exptl_crystal_description       sphere
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         2.567
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.442
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0829
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1494P)^2^+2.2142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2175
_refine_ls_wR_factor_ref         0.2197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4224
_reflns_number_total             4450
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra03563a2.cif
_cod_data_source_block           2H
_cod_database_code               7248858
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo8 C26 N6 O27'
_shelx_estimated_absorpt_t_max   0.826
_shelx_estimated_absorpt_t_min   0.267
_diffrn_oxdiff_digest_frames
;
0132248c46386eb3029e463f7ef6a1115204102a42a
;
_diffrn_oxdiff_digest_hkl
;
01555f63190e4857330c8c4486ef0a1ec71366
;
_reflns_odcompleteness_completeness 99.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.075) H5(0.065) H7(0.062) H10(0.066) H6(0.063) H3A(0.065)
 H12(0.073) H11(0.08) H13(0.066) H14A(0.091) H14B(0.091) H14C(0.091)
 Fixed X: O10(0.5) H3(1.036632) H5(0.517096) H7(0.731182) H10(0.949)
 H6(0.623672) H3A(0.664051) H12(1.218237) H11(1.174006) H13(1.127788)
 H14A(0.461543) H14B(0.342845) H14C(0.325488)
 Fixed Y: O10(0.5) H3(-0.083818) H5(0.726253) H7(0.418916) H10(0.123049)
 H6(0.528792) H3A(1.008752) H12(0.144765) H11(-0.081321) H13(0.365828)
 H14A(0.949789) H14B(1.065909) H14C(0.892077)
 Fixed Z: O10(1) H3(0.800341) H5(0.309421) H7(0.540894) H10(0.709134)
 H6(0.403621) H3A(0.444643) H12(0.942127) H11(0.911541) H13(0.853857)
 H14A(0.208531) H14B(0.254524) H14C(0.318187)
;
_shelx_res_checksum              36943
_shelx_hkl_checksum              78411
_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 2.279
_oxdiff_exptl_absorpt_empirical_full_min 0.353