Record-Large Indium-Oxo Clusters: Synthesis, Hierarchical Assembly, and Efficient Optical Limiting
Wang, Xiuzhen; Chen, Yian; Yi, Xiaofeng; Chen, Shumei; Zhang, Jian; Chemical Science  (2026) –; doi:10.1039/D6SC00913A

data_1576883
_publ_section_title
;
 Record-large indium-oxo clusters: synthesis, hierarchical assembly, and
 efficient optical limiting.
;
_journal_issue                   18
_journal_name_full               'Chemical science'
_journal_page_first              9256
_journal_page_last               9263
_journal_paper_doi               10.1039/d6sc00913a
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety
'C134.856 H211.712 Cl1.62 In30 N22.38 O91.14, 1.144(H2 O), 20[CH4O], 10.8[C6H15NO3]'
_chemical_formula_sum            'C219.66 H456 Cl1.62 In30 N33.18 O144.68'
_chemical_formula_weight         9379.51
_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   mixed
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2pw2sg
_audit_creation_date             2026-03-12
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-03-12 deposited with the CCDC.	2026-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                106.7630(10)
_cell_angle_beta                 102.0270(10)
_cell_angle_gamma                109.5980(10)
_cell_formula_units_Z            1
_cell_length_a                   15.3165(2)
_cell_length_b                   22.1037(3)
_cell_length_c                   24.5398(3)
_cell_measurement_reflns_used    78360
_cell_measurement_temperature    99.98(13)
_cell_measurement_theta_max      56.2920
_cell_measurement_theta_min      1.9850
_cell_volume                     7052.38(19)
_computing_cell_refinement       'CrysAlisPro 1.171.43.131a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.131a 64-bit (release 19-07-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.131a (Rigaku OD, 2024)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -66.00   6.00   0.50    0.24    --  -66.56  57.00 150.00  144
  2  \w    -66.00   6.00   0.50    0.24    --  -66.56  57.00 150.00  144
  3  \w    -56.00   4.00   0.50    0.24    --  -66.56  57.00   0.00  120
  4  \w    -51.00   6.00   0.50    0.24    --  -66.56  45.00  -8.00  114
  5  \w    -59.00 -12.00   0.50    0.24    --  -66.56  57.00 120.00   94
  6  \w    -43.00 -18.00   0.50    0.24    --  -66.56  38.00 120.00   50
  7  \w    -16.00  71.00   0.50    0.06    --   -1.41  45.00  -8.00  174
  8  \w    -22.00   3.00   0.50    0.24    --  -66.56  19.00 150.00   50
  9  \w    -43.00   7.00   0.50    0.24    --  -66.56  38.00  90.00  100
 10  \w    -43.00   7.00   0.50    0.24    --  -66.56  38.00 -60.00  100
 11  \w    -31.00  -5.00   0.50    0.24    --  -66.56  57.00-150.00   52
 12  \w    -66.00 -39.00   0.50    0.24    --  -66.56  57.00-150.00   54
 13  \w   -139.00 -52.00   0.50    0.24    --  -66.56 -45.00-158.00  174
 14  \w    -74.00  13.00   0.50    0.06    --   -1.41 -45.00-158.00  174
 15  \w   -111.00 -20.00   0.50    0.24    --  -66.56 125.00   0.00  182
 16  \w   -111.00 -25.00   0.50    0.24    --  -66.56 125.00 -60.00  172
 17  \w    -74.00  15.00   0.50    0.06    --   -1.41 -57.00  60.00  178
 18  \w    -74.00  15.00   0.50    0.06    --   -1.41 -57.00  60.00  178
 19  \w    -12.00  26.00   0.50    0.24    --   63.75 -19.00-120.00   76
 20  \w    -12.00  26.00   0.50    0.24    --   63.75 -19.00  30.00   76
 21  \w     49.00 136.00   0.50    0.24    --   63.75  45.00  -8.00  174
 22  \w     40.00 137.00   0.50    0.24    --   63.75  77.00 -90.00  194
 23  \w     -9.00  51.00   0.50    0.24    --   63.75 -45.00-158.00  120
 24  \w     -7.00  97.00   0.50    0.24    --   63.75 -99.00-150.00  208
 25  \w     -7.00  97.00   0.50    0.24    --   63.75 -99.00-150.00  208
 26  \w     20.00 111.00   0.50    0.24    --   63.75-125.00-150.00  182
 27  \w     20.00 111.00   0.50    0.24    --   63.75-125.00   0.00  182
 28  \w     20.00 111.00   0.50    0.24    --   63.75-125.00  90.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0671704000
_diffrn_orient_matrix_UB_12      0.0599840000
_diffrn_orient_matrix_UB_13      0.0040138000
_diffrn_orient_matrix_UB_21      0.0384334000
_diffrn_orient_matrix_UB_22      -0.0354865000
_diffrn_orient_matrix_UB_23      -0.0339610000
_diffrn_orient_matrix_UB_31      -0.0611384000
_diffrn_orient_matrix_UB_32      -0.0039652000
_diffrn_orient_matrix_UB_33      -0.0499859000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            133913
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         56.341
_diffrn_reflns_theta_min         2.002
_diffrn_source                   'Ga K\a'
_exptl_absorpt_coefficient_mu    13.912
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.131a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.208
_exptl_crystal_description       block
_exptl_crystal_F_000             4661
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.184
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1318
_refine_ls_number_reflns         27675
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+8.2573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0895
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22917
_reflns_number_total             27675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc00913a2.cif
_cod_data_source_block           InOC-41_auto
_cod_depositor_comments
'Adding full bibliography for 1576882--1576886.cif.'
_cod_original_cell_volume        7052.37(17)
_cod_database_code               1576883
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N In'
_chemical_oxdiff_usercomment     'C H O N In'
_cell_oxdiff_angle_alpha         106.7633(11)
_cell_oxdiff_angle_beta          102.0271(10)
_cell_oxdiff_angle_gamma         109.5978(11)
_cell_oxdiff_length_a            15.31651(19)
_cell_oxdiff_length_b            22.1037(3)
_cell_oxdiff_length_c            24.5398(3)
_cell_oxdiff_measurement_reflns_used 78360
_cell_oxdiff_volume              7052.37(15)
_shelx_estimated_absorpt_t_max   0.337
_shelx_estimated_absorpt_t_min   0.167
_diffrn_oxdiff_digest_hkl
;
01b5abc39fc89e10d3ddb2f8a098141e9bd222
;
_olex2_refinement_description
;
1. Restrained distances
 C68A-C38
 1.4 with sigma of 0.01
 O1-N48 = O65-N48 = O49-N48
 1.17 with sigma of 0.02
 C68A-O36
 1.35 with sigma of 0.01
 O65-O1 = O65-O49 = O1-O49
 2.18 with sigma of 0.02
 In15-O65
 2.1 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
C68 \\sim C68A \\sim C38 \\sim O36: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Cl2 \\sim O49 \\sim N48 \\sim O1 \\sim O65: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002 within 2A
3. Others
 Sof(H38C)=Sof(H38D)=Sof(C68A)=Sof(H68C)=Sof(H68D)=1-FVAR(1)
 Sof(H38A)=Sof(H38B)=Sof(C68)=Sof(H68A)=Sof(H68B)=FVAR(1)
 Fixed Sof: H20(0.572) C69(0.428) H69A(0.428) H69B(0.428) H69C(0.428)
 O47(0.572) H47C(0.572) H47D(0.572) Cl2(0.81) O49(0.19) N48(0.19) O1(0.19)
 O65(0.19)
4.a Riding coordinates:
 O20(H20), O26(H26), O42(H42), O44(H44), O45(H45), O46(H46), O47(H47C,H47D)
4.b Ternary CH refined with riding coordinates:
 O15(H15)
4.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A,
 H16B), C18(H18A,H18B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B),
 C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
  C29(H29A,H29B), C32(H32A,H32B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,
 H36B), C37(H37A,H37B), C38(H38A,H38B), C38(H38C,H38D), C41(H41A,H41B),
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
  C48(H48A,H48B), C49(H49A,H49B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,
 H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B),
 C60(H60A,H60B), C61(H61A,H61B), C63(H63A,H63B), C65(H65A,H65B), C66(H66A,H66B),
  C68(H68A,H68B), C68A(H68C,H68D)
4.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C8(H8), C9(H9), C15(H15A), C30(H30), C51(H51), C59(H59),
 C62(H62), C64(H64)
4.e Tetrahedral OH refined with riding coordinates:
 O38(H38)
4.f Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C69(H69A,H69B,H69C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1237 electrons were 
found in a volume of 2931\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
20[CH4O], 10.8[C6H15NO3] per Asymmetric Unit 
which account for 1246 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.0
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              53527
_shelx_fab_checksum              73484
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.922
_oxdiff_exptl_absorpt_empirical_full_min 0.651