Photoabsorption of 1–2 nm molecular Ce-oxo nanoclusters versus ceria: intervalence charge transfer but no size effects
Brown, Stephen E.; Pike, Sebastian D.; Chemical Science 16 (2025) 11659–11668; doi:10.1039/D5SC00905G

data_1574753
_publ_section_title
;
 Photoabsorption of 1--2 nm molecular Ce-oxo nanoclusters versus ceria:
 intervalence charge transfer but no size effects
;
_journal_issue                   25
_journal_name_full               'Chemical Science'
_journal_page_first              11659
_journal_page_last               11668
_journal_paper_doi               10.1039/D5SC00905G
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C315 H287 Ce24 N15 O126'
_chemical_formula_sum            'C315 H287 Ce24 N15 O126'
_chemical_formula_weight         9661.65
_chemical_melting_point          ?
_chemical_name_systematic        '[Ce24O28(OH)8(OOCC6H4(4-OMe))30(py)4](py)11'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2025-01-20
_audit_creation_method           CRYSTALS_ver_14.61_build_6999
_audit_update_record
;
2025-01-21 deposited with the CCDC.	2025-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.700(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   36.1757(6)
_cell_length_b                   25.1668(4)
_cell_length_c                   42.5226(8)
_cell_measurement_reflns_used    86821
_cell_measurement_temperature    100
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     36214.5(12)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_av_unetI/netI     0.066
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            299949
_diffrn_reflns_theta_full        25.004
_diffrn_reflns_theta_max         26.320
_diffrn_reflns_theta_min         2.077
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.033
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.30
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             18728
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.098
_platon_squeeze_details
;
44 solvent pyridines in 4 pores , electron count and 
volume consistent with proposed solvent 
;
_refine_diff_density_max         9.10
_refine_diff_density_min         -9.79
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.7423
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4321
_refine_ls_number_reflns         65029
_refine_ls_number_restraints     2943
_refine_ls_R_factor_all          0.1467
_refine_ls_R_factor_gt           0.1024
_refine_ls_shift/su_max          0.3033028
_refine_ls_shift/su_mean         0.0045172
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.20P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.4361
_refine_ls_wR_factor_gt          0.3745
_refine_ls_wR_factor_ref         0.4361
_reflns_limit_h_max              41
_reflns_limit_h_min              -44
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              52
_reflns_limit_l_min              0
_reflns_number_gt                40779
_reflns_number_total             65059
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.62
_oxford_diffrn_Wilson_scale      949.43
_oxford_refine_ls_r_factor_ref   0.1467
_oxford_refine_ls_scale          0.035551(6)
_oxford_reflns_number_all        65030
_oxford_structure_analysis_title 'perstructure\sb3.88.cif_od At 13:50 on 19/10'
_cod_data_source_file            d5sc00905g2.cif
_cod_data_source_block           ce24PhOMe
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

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 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1574748--1574755.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               1574753
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_platon_squeeze_void_probe_radius 1.20