Timing matters: pre-assembly versus post-assembly functionalization of a polyoxovanadate–organic cuboid
Guo, Ji; Liu, Junrui; Cui, Yingcui; Liu, Chuanhong; Wang, Yangming; Wang, Mou; Huang, Danmeng; Chen, Guanying; Wang, Wei; Xia, Debin; Fang, Xikui; Chemical Science  (2022) –; doi:10.1039/D2SC00533F

data_1566797
_publ_section_title
;
 Timing matters: pre-assembly versus post-assembly functionalization of a
 polyoxovanadate--organic cuboid
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC00533F
_journal_year                    2022
_chemical_formula_sum            'C423 H697 N33 O273 S8 V54'
_chemical_formula_weight         13620.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-01-26 deposited with the CCDC.	2022-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                113.872(2)
_cell_angle_beta                 92.142(2)
_cell_angle_gamma                103.627(2)
_cell_formula_units_Z            1
_cell_length_a                   20.5891(17)
_cell_length_b                   28.609(2)
_cell_length_c                   33.168(3)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.84
_cell_measurement_theta_min      2.29
_cell_volume                     17168(2)
_computing_cell_refinement       'Bruker APEX3'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker APEX3'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker PHOTON II detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0986
_diffrn_reflns_av_unetI/netI     0.1226
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            236288
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.433
_diffrn_reflns_theta_min         2.141
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker APEX3'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7020
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.600
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.667
_refine_diff_density_min         -3.731
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1728
_refine_ls_number_reflns         70399
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.2529
_refine_ls_R_factor_gt           0.1495
_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^)+(0.0936P)^2^+235.9704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3398
_refine_ls_wR_factor_ref         0.4042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30665
_reflns_number_total             70399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00533f2.cif
_cod_data_source_block           gj_1_sq
_cod_database_code               1566797
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.644
_shelx_estimated_absorpt_t_max   0.795
_exptl_absorpt_special_details   SADABS-2012/1
_shelx_res_checksum              43155
_shelx_hkl_checksum              71800
_shelx_fab_checksum              53394