Epoxidation vs. dehydrogenation of allylic alcohols: Heterogenization of the VO(acac)2 catalyst in a metal-organic framework
Negro, Cristina; Bilanin Artigado, Cristina; Qu, Xiaoni; Oliver-Meseguer, Judit; Ferrando-Soria, Jesús; Leyva-Perez, Antonio; Armentano, Donatella; Pardo, Emilio; Chemical Communications  (2022) –; doi:10.1039/D2CC01137A

data_7129930
_publ_section_title
;
 Epoxidation vs. dehydrogenation of allylic alcohols: Heterogenization of
 the VO(acac)2 catalyst in a metal-organic framework
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01137A
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_sum            'C41 H77 Ca Cu6 N6 O33 S6 V'
_chemical_formula_weight         1846.70
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-02-24 deposited with the CCDC.	2022-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   17.8884(17)
_cell_length_b                   17.8884(17)
_cell_length_c                   12.8853(13)
_cell_measurement_reflns_used    4032
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      22.8
_cell_measurement_theta_min      2.27
_cell_volume                     3570.8(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1168
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            41658
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.175
_diffrn_reflns_theta_min         2.277
_exptl_absorpt_coefficient_mu    2.211
_exptl_absorpt_correction_T_max  0.782
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green-blue
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       prism
_exptl_crystal_F_000             1884
_exptl_crystal_recrystallization_method
'Single crystal to single crystal process'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.441
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.176
_refine_ls_abs_structure_details
;
 Flack x determined using 1060 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.20(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4766
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.0775
_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^)+(0.1383P)^2^+13.2742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2076
_refine_ls_wR_factor_ref         0.2493
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                2967
_reflns_number_total             4766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01137a2.cif
_cod_data_source_block           X6_0m
_cod_original_cell_volume        3570.8(8)
_cod_database_code               7129930
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              73986