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_7248861
_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(C17 H18 Mo N3 O6), 2(C3 H6 O)'
_chemical_formula_sum            'C40 H48 Mo8 N6 O33'
_chemical_formula_weight         1908.36
_chemical_name_systematic
'[N'-(2-oxo-3-methoxybenzylidene)nicotinoylhydrazonium](acetone)dioxomolybdenum(vi) hexamolybdate acetone solvate'
_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             2022-04-27
_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                104.858(2)
_cell_angle_beta                 104.620(2)
_cell_angle_gamma                94.020(2)
_cell_formula_units_Z            1
_cell_length_a                   8.9721(3)
_cell_length_b                   10.7368(2)
_cell_length_c                   16.4964(4)
_cell_measurement_reflns_used    14257
_cell_measurement_temperature    169.99
_cell_measurement_theta_max      80.0670
_cell_measurement_theta_min      2.8910
_cell_volume                     1470.73(7)
_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      169.99
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.939
_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     69.00  97.00   0.50    0.05    --   48.02  52.00  97.00   56
  2  \w    138.00 165.00   0.50    0.19    --  113.25  61.00  30.00   54
  3  \w    102.00 151.00   0.50    0.19    --  113.25  45.00   0.00   98
  4  \w    103.00 133.00   0.50    0.19    --  113.25  61.00  30.00   60
  5  \w     99.00 175.00   0.50    0.19    --  113.25  61.00  60.00  152
  6  \w    114.00 178.00   0.50    0.19    --  113.25  52.00  97.00  128
  7  \w    126.00 175.00   0.50    0.19    --  113.25  45.00 120.00   98
  8  \w    142.00 172.00   0.50    0.19    --  113.25  30.00 150.00   60
  9  \w    101.00 149.00   0.50    0.19    --  113.25  45.00  90.00   96
 10  \w    114.00 158.00   0.50    0.19    --  113.25  30.00   0.00   88
 11  \w    113.00 144.00   0.50    0.19    --  113.25  30.00 -90.00   62
 12  \w    138.00 172.00   0.50    0.19    --  113.25  45.00-150.00   68
 13  \w    144.00 173.00   0.50    0.19    --  113.25  15.00-150.00   58
 14  \w    115.00 141.00   0.50    0.19    --  113.25  15.00-150.00   52
 15  \w    -20.00  25.00   0.50    0.05    --   48.02 -19.00-150.00   90
 16  \w    -21.00  59.00   0.50    0.05    --   48.02 -52.00 -47.00  160
 17  \w    -12.00  63.00   0.50    0.05    --   48.02 -57.00  90.00  150
 18  \w     42.00 109.00   0.50    0.19    --  113.25-125.00  60.00  134
 19  \w     93.00 118.00   0.50    0.19    --  113.25-134.00   1.06   50
 20  \w     46.00  72.00   0.50    0.19    --  113.25-134.00   1.06   52
 21  \w     85.00 111.00   0.50    0.19    --  113.25-125.00 -90.00   52
 22  \w     62.00 111.00   0.50    0.19    --  113.25-125.00-150.00   98
 23  \w     43.00  78.00   0.50    0.19    --  113.25-125.00-180.00   70
 24  \w     84.00 111.00   0.50    0.19    --  113.25-125.00-180.00   54
 25  \w     35.00  96.00   0.50    0.05    --   48.02-125.00 -30.00  122
 26  \w     69.00 110.00   0.50    0.19    --  113.25-125.00  90.00   82
 27  \w     84.00 110.00   0.50    0.19    --  113.25-125.00 150.00   52
 28  \w     45.00 104.00   0.50    0.19    --  113.25 -95.00  60.00  118
 29  \w     64.00 108.00   0.50    0.19    --  113.25-110.00  18.97   88
 30  \w     77.00 102.00   0.50    0.19    --  113.25 -95.00   0.00   50
 31  \w     42.00  69.00   0.50    0.19    --  113.25-108.00-100.20   54
 32  \w     45.00  79.00   0.50    0.19    --  113.25 -99.00-150.56   68
 33  \w     80.00 107.00   0.50    0.19    --  113.25-108.00-100.20   54
 34  \w     71.00 102.00   0.50    0.19    --  113.25 -95.00 -90.00   62
 35  \w     54.00 104.00   0.50    0.19    --  113.25 -95.00 -60.00  100
 36  \w     43.00  96.00   0.50    0.19    --  113.25 -95.00  90.00  106
 37  \w     46.00  71.00   0.50    0.19    --  113.25 -61.00  90.00   50
 38  \w     56.00  88.00   0.50    0.19    --  113.25 -77.00  90.00   64
 39  \w     73.00 101.00   0.50    0.19    --  113.25 -77.00 -60.00   56
 40  \w     44.00  69.00   0.50    0.19    --  113.25 -77.00 -60.00   50
 41  \w     43.00  69.00   0.50    0.19    --  113.25 -61.00 -60.00   52
 42  \w     44.00  70.00   0.50    0.19    --  113.25 -77.00-120.00   52
 43  \w     45.00  70.00   0.50    0.19    --  113.25 -61.00-120.00   50
 44  \w     42.00  68.00   0.50    0.19    --  113.25 -61.00 -90.00   52
 45  \w     42.00  68.00   0.50    0.19    --  113.25 -61.00 150.00   52
 46  \w    114.00 167.00   0.50    0.19    --  113.25 125.00 -90.00  106
 47  \w     96.00 140.00   0.50    0.19    --  113.25 125.00 -30.00   88
 48  \w    150.00 176.00   0.50    0.19    --  113.25 125.00 -30.00   52
 49  \w    -20.00  23.00   0.50    0.05    --  -48.02  52.00  97.00   86
 50  \w    -53.00 -23.00   0.50    0.05    --  -48.02  52.00  97.00   60
 51  \w    -56.00 -31.00   0.50    0.19    --  -91.75  52.00  97.00   50
 52  \w    -70.00 -22.00   0.50    0.19    --  -91.75  61.00 -90.00   96
 53  \w    -46.00 -21.00   0.50    0.19    --  -91.75  45.00-120.00   50
 54  \w    -51.00 -21.00   0.50    0.19    --  -91.75  45.00-150.00   60
 55  \w   -118.00 -65.00   0.50    0.05    --  -48.02 -52.00 -47.00  106
 56  \w   -120.00 -95.00   0.50    0.05    --  -48.02-125.00 -60.00   50
 57  \w   -119.00 -81.00   0.50    0.05    --  -48.02-125.00-120.00   76
 58  \w   -121.00 -96.00   0.50    0.19    --  -91.75 -52.00 -47.00   50
 59  \w   -111.00 -76.00   0.50    0.05    --  -48.02-125.00  90.00   70
;
_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      0.0846773000
_diffrn_orient_matrix_UB_12      0.0515922000
_diffrn_orient_matrix_UB_13      -0.0578610000
_diffrn_orient_matrix_UB_21      -0.1360409000
_diffrn_orient_matrix_UB_22      0.0743879000
_diffrn_orient_matrix_UB_23      -0.0272258000
_diffrn_orient_matrix_UB_31      0.0804999000
_diffrn_orient_matrix_UB_32      0.1196205000
_diffrn_orient_matrix_UB_33      0.0777350000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18183
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.522
_diffrn_reflns_theta_min         2.887
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.380
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.194
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.155
_exptl_crystal_description       plate
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.002
_refine_diff_density_max         2.389
_refine_diff_density_min         -2.465
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       0.00063(9)
_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   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         6056
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0647P)^2^+5.8824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5659
_reflns_number_total             6056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra03563a2.cif
_cod_data_source_block           1Ha-2CH3COCH3
_cod_database_code               7248861
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mo4 O17 C18 N3'
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.157
_diffrn_oxdiff_digest_frames
;
017a254803ed035e4dbb6c008c31acfcde04474c95e
;
_diffrn_oxdiff_digest_hkl
;
011e8965894199009e7d02648f50bc13e049c5
;
_reflns_odcompleteness_completeness 96.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Others
 Fixed Sof: C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C19(0.5) H19A(0.5)
 H19B(0.5) H19C(0.5)
 Fixed Uiso: H3(0.029) H7(0.028) H10(0.029) H6(0.032) H13(0.03) H11(0.033)
 H4(0.044) H5(0.04) H12(0.034) H16A(0.065) H16B(0.065) H16C(0.065) H17A(0.049)
 H17B(0.049) H17C(0.049) H20A(0.085) H20B(0.085) H20C(0.085) H14A(0.103)
 H14B(0.103) H14C(0.103) H21A(0.074) H21B(0.074) H21C(0.074) H19A(0.131)
 H19B(0.131) H19C(0.131)
 Fixed X: O11(0) H3(0.558754) H7(0.229358) H10(0.458911) H6(0.10687)
 H13(0.548532) H11(0.651168) H4(-0.008301) H5(-0.004699) H12(0.645205)
 H16A(0.306313) H16B(0.165058) H16C(0.18645) H17A(-0.119318) H17B(-0.075916)
 H17C(-0.123387) H20A(0.438) H20B(0.479433) H20C(0.615203) H14A(-0.068009)
 H14B(0.099195) H14C(0.052487) H21A(0.293833) H21B(0.236462) H21C(0.291663)
 H19A(0.614686) H19B(0.430426) H19C(0.525722)
 Fixed Y: O11(0.5) H3(0.859616) H7(1.037632) H10(0.907202) H6(1.175552)
 H13(0.55662) H11(0.676219) H4(1.067475) H5(1.216396) H12(0.516605)
 H16A(0.453075) H16B(0.358838) H16C(0.360837) H17A(0.411712) H17B(0.463517)
 H17C(0.561314) H20A(1.269152) H20B(1.266134) H20C(1.274673) H14A(0.872545)
 H14B(0.94226) H14C(0.788361) H21A(0.948473) H21B(1.072127) H21C(1.079801)
 H19A(1.098304) H19B(1.065962) H19C(0.956217)
 Fixed Z: O11(0) H3(0.182985) H7(0.480085) H10(0.296871) H6(0.574798)
 H13(0.3314) H11(0.13596) H4(0.770846) H5(0.689281) H12(0.208366)
 H16A(0.415659) H16B(0.340031) H16C(0.43967) H17A(0.370518) H17B(0.295446)
 H17C(0.372769) H20A(0.208933) H20B(0.119671) H20C(0.205973) H14A(0.799923)
 H14B(0.863792) H14C(0.842625) H21A(0.130374) H21B(0.10105) H21C(0.202561)
 H19A(0.05337) H19B(0.009922) H19C(0.03832)
;
_shelx_res_checksum              37050
_shelx_hkl_checksum              4646
_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 2.603
_oxdiff_exptl_absorpt_empirical_full_min 0.639