Cerium-Oxo clusters for photocatalytic aerobic oxygenation of sulfides to sulfoxides
Lv, Xinjie; Zhao, Xiao-li; Zhao, Qixin; Zheng, Qi; Xuan, Weimin; Dalton Transactions  (2022) –; doi:10.1039/D2DT00856D

data_7710342
_publ_section_title
;
 Cerium-Oxo clusters for photocatalytic aerobic oxygenation of sulfides to
 sulfoxides
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00856D
_journal_year                    2022
_chemical_formula_moiety
'C144 H104 Ce16 N24 O75, 20[C5H5N], 30[C2H3N], 60[H2O]'
_chemical_formula_sum            'C304 H414 Ce16 N74 O135'
_chemical_formula_weight         9506.99
_space_group_crystal_system      cubic
_space_group_IT_number           215
_space_group_name_Hall           'P -4 2 3'
_space_group_name_H-M_alt        'P -4 3 m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-05-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-05-22 deposited with the CCDC.	2022-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   18.9003(8)
_cell_length_b                   18.9003(8)
_cell_length_c                   18.9003(8)
_cell_measurement_reflns_used    9830
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      24.73
_cell_measurement_theta_min      2.27
_cell_volume                     6751.6(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       HKL3000
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
Shanghai Synchrotron Radiation Facility, beam line station 
BL17B, Bruker/ARINAX MD2 equipped with a MarCCD-300 detector
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.67011
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            86270
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        23.707
_diffrn_reflns_theta_max         24.756
_diffrn_reflns_theta_min         1.760
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    2.383
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.4304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1869 before and 0.0831 after correction.
The Ratio of minimum to maximum transmission is 0.5776.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    2.338
_exptl_crystal_description       block
_exptl_crystal_F_000             4764
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.624
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.43(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2625
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0696P)^2^+21.6207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1163
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2534
_reflns_number_total             2625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00856d2.cif
_cod_data_source_block           p-43m
_cod_original_cell_volume        6751.6(9)
_cod_database_code               7710342
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.779
_shelx_estimated_absorpt_t_min   0.716
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.57(7)
 0.43(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 C8-C9 = C9-C10 = C10_$1-C9_$1 = C9_$1-C8
 1.39 with sigma of 0.005
 C10-N2 = N2-C10_$1
 1.34 with sigma of 0.005
 C1-C2
 1.5 with sigma of 0.02
 C8-C7
 1.51 with sigma of 0.02
 O9-C7 = O8-C7
 1.25 with sigma of 0.02
 O6-C1
 1.25 with sigma of 0.02
4. Restrained planarity
 O9, C8, C9, C10, N2, C10_$1, C9_$1
 with sigma of 0.1
 C7, C8, C9, C10, N2, C12, C11
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(O9) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(N2) \\sim
Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
7. Others
 Fixed Sof: H3B(0.16667) H3A(0.16667) O6(0.5) O7(0.5) O8(0.5) C1(0.5) C2(0.5)
 C3(0.5) H3(0.5) C4(0.5) H4(0.5) N1(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5)
 O9(0.5) N2(0.5) C10(0.5) H10(0.5) C9(0.5) H9(0.5) C12(0.5) H12(0.5) C11(0.5)
 H11(0.5) C7(0.5)
8.a Riding coordinates:
 O3(H3B,H3A)
8.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C9(H9), C12(H12), C11(H11)
8.c Fitted hexagon refined as free rotating group:
 C2(C3,C4,N1,C5,C6), N2(C10,C9,C8,C12,C11)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 2034 electrons were 
found in a volume of 2411\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
20[C5H5N], 30[C2H3N], 60[H2O] per Unit Cell 
which account for 2100 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              95833
_shelx_hkl_checksum              96459
_shelx_fab_checksum              99252
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'