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_7248859
_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         'C28 H24 Mo8 N6 O29'
_chemical_formula_sum            'C28 H24 Mo8 N6 O29'
_chemical_formula_weight         1676.05
_chemical_name_systematic
(u6-oxo)-tetradecakis(u2-oxo)-octaoxo-bis(N-(2-oxy-3-(methoxy)benzylidene)nicotinylhydrazonato)-octa-molybdenum
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-13
_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                90.460(5)
_cell_angle_beta                 92.740(5)
_cell_angle_gamma                108.443(5)
_cell_formula_units_Z            1
_cell_length_a                   10.0670(6)
_cell_length_b                   10.0808(6)
_cell_length_c                   11.2764(7)
_cell_measurement_reflns_used    2821
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.4940
_cell_measurement_theta_min      4.2710
_cell_volume                     1084.03(12)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_details
;
  1 omega  -43.00   -1.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432  -77.0000  -90.0000 42

  2 omega  -44.00    1.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432  -77.0000 -180.0000 45

  3 omega    7.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   77.0000   30.0000 82

  4 omega   -3.00   72.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   77.0000 -150.0000 75

  5 omega   -6.00   59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432  -99.0000  120.0000 65

  6 omega   35.00   84.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432  179.0000  120.0000 49

  7 omega    1.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   77.0000  -60.0000 86

  8 omega  -75.00  -49.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4994  179.0000  -30.0000 26

  9 omega  -17.00    8.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4994   19.0000    0.0000 25

 10 omega  -48.00  -22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4994   19.0000    0.0000 26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0625542000
_diffrn_orient_matrix_UB_12      0.0577020000
_diffrn_orient_matrix_UB_13      0.0061131000
_diffrn_orient_matrix_UB_21      0.0395283000
_diffrn_orient_matrix_UB_22      -0.0465718000
_diffrn_orient_matrix_UB_23      0.0084297000
_diffrn_orient_matrix_UB_31      0.0075162000
_diffrn_orient_matrix_UB_32      -0.0024789000
_diffrn_orient_matrix_UB_33      -0.0621255000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_unetI/netI     0.1572
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15537
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.002
_diffrn_reflns_theta_min         4.104
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.343
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86769
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.567
_exptl_crystal_description       plate
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.173
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         7115
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.1312
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0090P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4159
_reflns_number_total             7115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra03563a2.cif
_cod_data_source_block           1H
_cod_database_code               7248859
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Mo
_chemical_oxdiff_usercomment     'zuta iglica 3py4OHsal'
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.615
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Restrained distances
 N3-H3
 0.82 with sigma of 0.02
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C5(H5), C11(H11), C13(H13), C4(H4), C10(H10), C12(H12)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              50948
_shelx_hkl_checksum              41355
_olex2_submission_special_instructions 'No special instructions were received'