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_7248865
_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         '4(C14 H14 Mo N3 O6), 2(Mo6 O19)'
_chemical_formula_sum            'C56 H56 Mo16 N12 O62'
_chemical_formula_weight         3424.16
_chemical_name_systematic
'bis((aquo)-dioxo-(N-(2-oxy-3-methoxybenzylidene)nicotinylhydrazonato)-molybdenum(vi)) hexamolybdate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-05-02
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
;
2024-02-27 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.717(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   11.2569(3)
_cell_length_b                   9.2706(2)
_cell_length_c                   21.2974(5)
_cell_measurement_reflns_used    6137
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.2690
_cell_measurement_theta_min      4.4450
_cell_volume                     2159.17(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_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      150
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_details
;
  1 omega    7.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4994   19.0000   60.0000 83

  2 omega   17.00   72.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4994   57.0000   90.0000 55

  3 omega   66.00   91.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4994  179.0000    0.0000 25

  4 omega  -33.00   -8.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4994  -57.0000   60.0000 25

  5 omega   23.00   59.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4994  -99.0000    0.0000 36

  6 omega  -34.00   24.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4994  -57.0000 -120.0000 58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0451
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_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15865
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.927
_diffrn_reflns_theta_min         4.327
_exptl_absorpt_coefficient_mu    2.359
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    2.633
_exptl_crystal_description       prism
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_parameters     348
_refine_ls_number_reflns         7131
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0265P)^2^+2.1483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                5735
_reflns_number_total             7131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra03563a2.cif
_cod_data_source_block           1Hw
_cod_database_code               7248865
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.852
_shelx_estimated_absorpt_t_min   0.781
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H10(0.024) H7(0.023) H12(0.031) H6(0.027) H14A(0.038) H14B(0.038)
 H14C(0.038) H4(0.027) H5(0.031) H13(0.027)
 Fixed X: O12(0) H10(0.101592) H7(0.463409) H12(0.170148) H6(0.594594)
 H14A(0.593776) H14B(0.631855) H14C(0.722606) H4(0.696157) H5(0.704385)
 H13(0.278077)
 Fixed Y: O12(0) H10(0.741329) H7(0.83823) H12(1.2337) H6(0.77506)
 H14A(0.130365) H14B(0.044834) H14C(0.16217) H4(0.361765) H5(0.606667)
 H13(1.081266)
 Fixed Z: O12(0.5) H10(0.800935) H7(0.624041) H12(0.796641) H6(0.555615)
 H14A(0.544321) H14B(0.611367) H14C(0.59331) H4(0.536868) H5(0.51096)
 H13(0.745377)
;
_shelx_res_checksum              71042
_shelx_hkl_checksum              39008
_olex2_submission_special_instructions 'No special instructions were received'