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_7248862
_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 H14 Mo N3 O6), 2(C3 H6 O)'
_chemical_formula_sum            'C34 H40 Mo8 N6 O33'
_chemical_formula_weight         1828.24
_chemical_name_systematic
'bis((aquo)-dioxo-(N-(2-oxy-3-methoxybenzylidene)nicotinylhydrazonato)-molybdenum(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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-05-02
_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                108.527(4)
_cell_angle_beta                 92.219(3)
_cell_angle_gamma                110.565(4)
_cell_formula_units_Z            1
_cell_length_a                   10.1475(4)
_cell_length_b                   10.3331(5)
_cell_length_c                   14.6331(5)
_cell_measurement_reflns_used    2947
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.1540
_cell_measurement_theta_min      4.4020
_cell_volume                     1342.45(11)
_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      150.0
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.983
_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  0.0540
_diffrn_reflns_av_unetI/netI     0.0874
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17550
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.000
_diffrn_reflns_theta_min         3.977
_exptl_absorpt_coefficient_mu    1.907
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    2.261
_exptl_crystal_description       plate
_exptl_crystal_F_000             886
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         7018
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0361P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4379
_reflns_number_total             7018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra03563a2.cif
_cod_data_source_block           2Hw-2CH3COCH3
_cod_database_code               7248862
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.832
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H7(0.044) H3(0.058) H3A(0.043) H13(0.053) H10(0.048) H5(0.049)
 H12(0.061) H14A(0.08) H14B(0.08) H14C(0.08) H11(0.066) H17A(0.096) H17B(0.096)
 H17C(0.096) H15A(0.154) H15B(0.154) H15C(0.154) H6A(0.051) H6B(0.051) H6(0.047)
 Fixed X: H7(0.434968) H3A(0.767833) H13(-0.004875) H10(-0.139395)
 H5(0.916918) H12(-0.241949) H14A(1.136023) H14B(0.996908) H14C(0.985292) H11(-
 0.422688) H17A(0.341548) H17B(0.347595) H17C(0.245302) H15A(0.523053)
 H15B(0.552492) H15C(0.651654) O11(1) H6(0.687405)
 Fixed Y: H7(0.160398) H3A(0.220495) H13(0.048573) H10(-0.059644) H5(0.330678)
 H12(-0.03911) H14A(0.355886) H14B(0.388645) H14C(0.221772) H11(-0.143816)
 H17A(0.443788) H17B(0.597827) H17C(0.52333) H15A(0.447752) H15B(0.53078)
 H15C(0.605228) O11(0.5) H6(0.260371)
 Fixed Z: H7(0.18402) H3A(0.49658) H13(0.102109) H10(0.332851) H5(0.268133)
 H12(0.028271) H14A(0.543041) H14B(0.570404) H14C(0.522537) H11(0.105587)
 H17A(0.33854) H17B(0.41373) H17C(0.309641) H15A(0.268916) H15B(0.191774)
 H15C(0.297065) O11(0) H6(0.192696)
;
_shelx_res_checksum              34163
_shelx_hkl_checksum              93360
_olex2_submission_special_instructions 'No special instructions were received'