Visible-light-responsive catalysis of a zinc-introduced lacunary disilicoicosatungstate for deoxygenation of pyridine N-oxides
Jeong, Jinu; Suzuki, Kosuke; Yamaguchi, Kazuya; Mizuno, Noritaka; New J. Chem. 41 (2017) 13226–13229; doi:10.1039/C7NJ03057F

data_7056681
_publ_section_title
;
 Visible-light-responsive catalysis of a zinc-introduced lacunary
 disilicoicosatungstate for deoxygenation of pyridine N-oxides
;
_journal_issue                   22
_journal_name_full               'New J. Chem.'
_journal_page_first              13226
_journal_page_last               13229
_journal_paper_doi               10.1039/C7NJ03057F
_journal_volume                  41
_journal_year                    2017
_chemical_formula_sum            'C128 N15 O69 Si2 W20 Zn'
_chemical_formula_weight         6649.98
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-10-06 deposited with the CCDC.
2017-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.4143(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   51.6192(4)
_cell_length_c                   20.9479(2)
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_cell_measurement_theta_min      0.789
_cell_volume                     19260.7(3)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.073
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_number            53499
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         29.568
_diffrn_reflns_theta_min         0.789
_exptl_absorpt_coefficient_mu    12.097
_exptl_absorpt_correction_T_max  0.088
_exptl_absorpt_correction_T_min  0.053
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL2000 DENZO SCALEPACK'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.293
_exptl_crystal_description       prism
_exptl_crystal_F_000             11852
_refine_diff_density_max         2.801
_refine_diff_density_min         -2.943
_refine_diff_density_rms         0.437
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1431
_refine_ls_number_reflns         53499
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0777
_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^)+(0.0405P)^2^+888.8659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.1910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                44894
_reflns_number_total             53499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj03057f1.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        19260.8(3)
_cod_database_code               7056681
_shelxl_version_number           2014/6
_shelx_res_checksum              90746