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_1566798
_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            'C462 H719 N29 O236 P8 S0 V48'
_chemical_formula_weight         13148.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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
;
2022-01-24 deposited with the CCDC.	2022-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.9190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   45.210(2)
_cell_length_b                   27.4006(14)
_cell_length_c                   55.215(4)
_cell_measurement_reflns_used    9708
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.46
_cell_measurement_theta_min      2.34
_cell_volume                     62525(6)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0507
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            172105
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        21.556
_diffrn_reflns_theta_max         21.556
_diffrn_reflns_theta_min         2.194
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.6009
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'Bruker APEX3'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             27224
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.320
_refine_diff_density_max         1.973
_refine_diff_density_min         -1.596
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1261
_refine_ls_number_reflns         35874
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1828
_refine_ls_R_factor_gt           0.1445
_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^)+(0.3684P)^2^+759.9775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4306
_refine_ls_wR_factor_ref         0.4952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25160
_reflns_number_total             35874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00533f2.cif
_cod_data_source_block           gj_2_sq
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1566798
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.719
_shelx_estimated_absorpt_t_max   0.787
_exptl_absorpt_special_details   SADABS-2012/1
_shelx_res_checksum              13575
_shelx_hkl_checksum              97748
_shelx_fab_checksum              10536