Synthesis and oxidation catalysis of a difluoride-incorporated polyoxovanadate and isolation of active vanadium alkylperoxo species
Kikukawa, Yuji; Sakamoto, Yui; Hirasawa, Hikari; Kurimoto, Yushi; Iwai, Hiroya; Hayashi, Yoshihito; Catalysis Science & Technology 12 (2022) 2438–2445; doi:10.1039/D1CY02103F

data_1565976
_publ_section_title
;
 Synthesis and oxidation catalysis of a difluoride-incorporated
 polyoxovanadate and isolation of active vanadium alkylperoxo species
;
_journal_issue                   8
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              2438
_journal_page_last               2445
_journal_paper_doi               10.1039/D1CY02103F
_journal_volume                  12
_journal_year                    2022
_chemical_formula_sum            'C59 H126 F2 N4 O34 V12'
_chemical_formula_weight         2084.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-12-21 deposited with the CCDC.	2022-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.9450(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7995(4)
_cell_length_b                   23.6442(5)
_cell_length_c                   20.9424(4)
_cell_measurement_reflns_used    9836
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      76.9394
_cell_measurement_theta_min      2.8196
_cell_volume                     8808.6(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service vV6.2.6'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            71563
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.351
_diffrn_reflns_theta_min         2.819
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    10.872
_exptl_absorpt_correction_T_max  0.2741
_exptl_absorpt_correction_T_min  0.254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4296
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.119
_refine_diff_density_max         1.151
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1175
_refine_ls_number_reflns         18248
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0514P)^2^+23.8925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13965
_reflns_number_total             18248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy02103f2.cif
_cod_data_source_block           V12-acac
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1565975--1565977.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1565976
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.255
_shelx_estimated_absorpt_t_max   0.358
_shelx_res_checksum              45848