Synthesis and catalysis of a Co13 disk surrounded by vanadium–oxygen crown
Kikukawa, Yuji; Yoshida, Isshin; Mitsuhashi, Ryoji; Yamane, Masaru; Hayashi, Yoshihito; New Journal of Chemistry 48 (2024) 15307–15312; doi:10.1039/D4NJ02900C

data_7063392
_publ_section_title
;
 Synthesis and catalysis of a Co13 disk surrounded by vanadium--oxygen
 crown
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15307
_journal_page_last               15312
_journal_paper_doi               10.1039/D4NJ02900C
_journal_volume                  48
_journal_year                    2024
_chemical_formula_sum            'C112 H206 Co13 N10 O92 S8 V24'
_chemical_formula_weight         5409.99
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-06-20 deposited with the CCDC.	2024-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   33.1589(6)
_cell_length_b                   33.1589(6)
_cell_length_c                   15.9534(3)
_cell_measurement_reflns_used    337
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      53.4397
_cell_measurement_theta_min      2.6358
_cell_volume                     15190.9(5)
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean dtprofit.ref
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Graphite Monochromator'
_diffrn_measurement_method       'Mercury (2x2 bin mode)'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41210
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.564
_diffrn_reflns_theta_min         2.665
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    18.403
_exptl_absorpt_correction_T_max  0.18
_exptl_absorpt_correction_T_min  0.13
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8145
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.690
_refine_diff_density_min         -1.639
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         6696
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0636
_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^)+(0.1203P)^2^+151.4551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1817
_refine_ls_wR_factor_ref         0.2004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5332
_reflns_number_total             6696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02900c2.cif
_cod_data_source_block           Co13
_cod_depositor_comments          'Adding full bibliography for 7063392.cif.'
_cod_original_cell_volume        15190.9(6)
_cod_database_code               7063392
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.134
_shelx_estimated_absorpt_t_max   0.183
_shelx_res_checksum              66582