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_1565977
_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            'C52 H117 F2 N3 O32 V12'
_chemical_formula_weight         1945.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.1990(4)
_cell_length_b                   21.6914(5)
_cell_length_c                   54.0590(12)
_cell_measurement_reflns_used    9435
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      65.6003
_cell_measurement_theta_min      3.1884
_cell_volume                     20167.8(8)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service vV6.2.0'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1527
_diffrn_reflns_av_unetI/netI     0.1114
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            148184
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        66.793
_diffrn_reflns_theta_max         66.793
_diffrn_reflns_theta_min         2.195
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    9.441
_exptl_absorpt_correction_T_max  0.436
_exptl_absorpt_correction_T_min  0.176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             8000
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Flack x determined using 8718 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1820
_refine_ls_number_reflns         35450
_refine_ls_number_restraints     289
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1321
_refine_ls_R_factor_gt           0.0905
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+173.5814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2017
_refine_ls_wR_factor_ref         0.2254
_reflns_Friedel_coverage         0.962
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                25514
_reflns_number_total             35450
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cy02103f2.cif
_cod_data_source_block           V12-OOtBu
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

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_database_code               1565977
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.170
_shelx_estimated_absorpt_t_max   0.490
_shelx_res_checksum              97545
_shelx_fab_checksum              43579