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_1576885
_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
'C85.3 H122.6 In15 N7 O45, C7 H6 O2, 1.49(H2 O), [+ solvents]'
_chemical_formula_sum            'C96.3 H147.58 In15 N7 O52.49'
_chemical_formula_weight         3965.53
_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     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2pw2th
_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                76.0650(10)
_cell_angle_beta                 87.6540(10)
_cell_angle_gamma                70.4950(10)
_cell_formula_units_Z            2
_cell_length_a                   15.6948(3)
_cell_length_b                   17.2125(2)
_cell_length_c                   24.8215(4)
_cell_measurement_reflns_used    59585
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.6420
_cell_measurement_theta_min      1.8730
_cell_volume                     6128.91(18)
_computing_cell_refinement       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.101a 64-bit (release 13-12-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_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 0.855
_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    -41.00  25.00   0.50    7.33    --   -9.69  98.00 150.00  132
  2  \w    -22.00  42.00   0.50    7.33    --    9.85 -98.00  43.00  128
  3  \w    -22.00  25.00   0.50    7.33    --    9.85  98.00 150.00   94
  4  \w     -3.00  83.00   0.50    7.33    --    9.85  38.00  90.00  172
  5  \w    -18.00  42.00   0.50    7.33    --    9.85 -99.00 -60.00  120
  6  \w     -5.00  77.00   0.50    7.33    --    9.85  57.00 150.00  164
  7  \w    -63.00  22.00   0.50    7.33    --    9.85 -19.00-180.00  170
  8  \w     17.00  43.00   0.50    7.33    --    9.85  57.00 -30.00   52
  9  \w    -62.00  32.00   0.50    7.33    --    9.85 -77.00 -30.00  188
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0230887000
_diffrn_orient_matrix_UB_12      -0.0440950000
_diffrn_orient_matrix_UB_13      0.0032539000
_diffrn_orient_matrix_UB_21      0.0144540000
_diffrn_orient_matrix_UB_22      0.0080059000
_diffrn_orient_matrix_UB_23      -0.0276204000
_diffrn_orient_matrix_UB_31      0.0395092000
_diffrn_orient_matrix_UB_32      0.0045575000
_diffrn_orient_matrix_UB_33      0.0097472000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            138764
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.594
_diffrn_reflns_theta_min         1.866
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.855
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.101a (Rigaku Oxford Diffraction, 2023)
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    2.149
_exptl_crystal_description       block
_exptl_crystal_F_000             3859
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.747
_refine_diff_density_min         -1.802
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1668
_refine_ls_number_reflns         38239
_refine_ls_number_restraints     1023
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+9.0601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30542
_reflns_number_total             38239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc00913a2.cif
_cod_data_source_block           InOC-38_auto
_cod_depositor_comments
'Adding full bibliography for 1576882--1576886.cif.'
_cod_original_cell_volume        6128.91(17)
_cod_original_formula_sum        'C96.30 H147.58 In15 N7 O52.49'
_cod_database_code               1576885
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N In'
_cell_oxdiff_angle_alpha         76.0648(12)
_cell_oxdiff_angle_beta          87.6536(14)
_cell_oxdiff_angle_gamma         70.4953(14)
_cell_oxdiff_length_a            15.6948(3)
_cell_oxdiff_length_b            17.2125(2)
_cell_oxdiff_length_c            24.8215(4)
_cell_oxdiff_measurement_reflns_used 59585
_cell_oxdiff_volume              6128.91(16)
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.972
_exptl_absorpt_special_details   A
_diffrn_oxdiff_digest_hkl
;
01ccb8413049f0a82629c7a1e50f09f71de918
;
_olex2_refinement_description
;
1. Restrained distances
 C60A-C52A
 1.5 with sigma of 0.02
 O42A-C60A
 1.2 with sigma of 0.02
 O45A-C60A
 1.3 with sigma of 0.02
 C74A-C63A
 1.5 with sigma of 0.02
 O46A-C63A
 1.3 with sigma of 0.02
 O47A-C63A
 1.2 with sigma of 0.02
 C40A-C14A
 1.5 with sigma of 0.02
 O41A-C14A
 1.3 with sigma of 0.02
 O32A-C14A
 1.2 with sigma of 0.02
 N7-C55 = N7-C55A = N7-C59A = N7-C59 = N7-C45A = N7-C45
 1.45 with sigma of 0.02
 C61-C45 = C61A-C45A = C68A-C55A = C68-C55 = C59A-C58A = C59-C58
 1.54 with sigma of 0.02
 O16-C68A = O16-C68 = O21-C58A = O21-C58 = O26-C61 = O26-C61A
 1.4 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
O32 \\sim O41 \\sim C14 \\sim C40 \\sim C47 \\sim C78 \\sim C86 \\sim C89 \\sim
C91 \\sim C40A \\sim C47A \\sim C78A \\sim C86A \\sim C89A \\sim C91A \\sim
O32A \\sim O41A \\sim C14A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O42 \\sim O45 \\sim C48 \\sim C49 \\sim C52 \\sim C60 \\sim C62 \\sim C66 \\sim
C79 \\sim O42A \\sim O45A \\sim C48A \\sim C49A \\sim C52A \\sim C60A \\sim
C62A \\sim C66A \\sim C79A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C83A \\sim C90A \\sim C92A \\sim C74A \\sim C88A \\sim C63A \\sim C85A \\sim
O46A \\sim O47A \\sim C83 \\sim O46 \\sim C63 \\sim O47 \\sim C74 \\sim C85
\\sim C90 \\sim C88 \\sim C92: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
N7 \\sim C55 \\sim C58 \\sim C59 \\sim C68 \\sim C55A \\sim C68A \\sim C59A
\\sim C58A \\sim C45 \\sim C61 \\sim C45A \\sim C61A \\sim O26 \\sim O16 \\sim
O21: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C91) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(O42A)=Sof(O45A)=Sof(H45C)=Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(H49A)=
 Sof(C52A)=Sof(C66A)=Sof(H66A)=Sof(C79A)=Sof(H79A)=Sof(C62A)=Sof(H62A)=
 Sof(C60A)=1-FVAR(1)
 Sof(O42)=Sof(O45)=Sof(H45)=Sof(C49)=Sof(H49)=Sof(C48)=Sof(H48)=Sof(C62)=
 Sof(H62)=Sof(C79)=Sof(H79)=Sof(C66)=Sof(H66)=Sof(C52)=Sof(C60)=FVAR(1)
 Sof(C90A)=Sof(H90A)=Sof(C92A)=Sof(H92A)=Sof(C88A)=Sof(H88A)=Sof(C85A)=
 Sof(H85A)=Sof(C74A)=Sof(C83A)=Sof(H83A)=Sof(O46A)=Sof(H46C)=Sof(C63A)=
 Sof(O47A)=1-FVAR(2)
 Sof(O46)=Sof(O47)=Sof(H47B)=Sof(C63)=Sof(C88)=Sof(H88)=Sof(C85)=Sof(H85)=
 Sof(C74)=Sof(C83)=Sof(H83)=Sof(C90)=Sof(H90)=Sof(C92)=Sof(H92)=FVAR(2)
 Sof(C86A)=Sof(H86A)=Sof(C78A)=Sof(H78A)=Sof(C47A)=Sof(H47A)=Sof(C40A)=
 Sof(C89A)=Sof(H89A)=Sof(C91A)=Sof(H91A)=Sof(O32A)=Sof(O41A)=Sof(C14A)=1-FVAR(3)
 Sof(O32)=Sof(O41)=Sof(C14)=Sof(C40)=Sof(C89)=Sof(H89)=Sof(C91)=Sof(H91)=
 Sof(C86)=Sof(H86)=Sof(C78)=Sof(H78)=Sof(C47)=Sof(H47)=FVAR(3)
 Sof(C55A)=Sof(H55C)=Sof(H55D)=Sof(C68A)=Sof(H68C)=Sof(H68D)=Sof(C59A)=
 Sof(H59C)=Sof(H59D)=Sof(C58A)=Sof(H58C)=Sof(H58D)=Sof(C45A)=Sof(H45D)=
 Sof(H45E)=Sof(C61A)=Sof(H61C)=Sof(H61D)=1-FVAR(4)
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C58)=Sof(H58A)=
 Sof(H58B)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(C68)=
 Sof(H68A)=Sof(H68B)=FVAR(4)
 Fixed Sof: H14(0.2) H18(0.5) C81(0.8) H81A(0.8) H81B(0.8) H81C(0.8) C18(0.5)
 H18A(0.5) H18B(0.5) H18C(0.5) O13(0.5) H13C(0.5) H13D(0.5) O48(0.2) H48B(0.2)
 H48C(0.2) O49(0.79) H49B(0.79) H49C(0.79)
 Fixed Y: C14(0.873311)
4.a Riding coordinates:
 O14(H14), O18(H18), O13(H13C,H13D), O48(H48B,H48C), O49(H49B,H49C)
4.b Ternary CH refined with riding coordinates:
 O12(H12)
4.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B),
  C16(H16A,H16B), C17(H17A,H17B), C93(H93A,H93B), C19(H19A,H19B), C20(H20A,
 H20B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C31(H31A,H31B), C32(H32A,H32B),
  C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C38(H38A,
 H38B), C39(H39A,H39B), C42(H42A,H42B), C44(H44A,H44B), C45(H45A,H45B),
 C46(H46A,H46B), C55(H55A,H55B), C56(H56A,H56B), C58(H58A,H58B), C59(H59A,H59B),
  C61(H61A,H61B), C65(H65A,H65B), C68(H68A,H68B), C55A(H55C,H55D), C68A(H68C,
 H68D), C59A(H59C,H59D), C58A(H58C,H58D), C45A(H45D,H45E), C61A(H61C,H61D)
4.d Aromatic/amide H refined with riding coordinates:
 O(H), C22(H22), C67(H67), C71(H71), C75(H75), C41(H41), C89(H89), C91(H91),
 C86(H86), C78(H78), C47(H47), C49(H49), C48(H48), C62(H62), C79(H79), C66(H66),
  C64(H64), C69(H69), C80(H80), C84(H84), C77(H77), C72(H72), C50(H50),
 C54(H54), C87(H87), C82(H82), C73(H73), C70(H70), C51(H51), C37(H37), C76(H76),
  C88(H88), C85(H85), C83(H83), C90(H90), C92(H92), C48A(H48A), C49A(H49A),
 C66A(H66A), C79A(H79A), C62A(H62A), C90A(H90A), C92A(H92A), C88A(H88A),
 C85A(H85A), C83A(H83A), C86A(H86A), C78A(H78A), C47A(H47A), C89A(H89A),
 C91A(H91A)
4.e Fitted hexagon refined as free rotating group:
 C4(C22,C67,C71,C75,C41), C40(C89,C91,C86,C78,C47), C49(C48,C62,C79,C66,C52),
 C64(C57,C69,C80,C84,C77), C72(C50,C43,C54,C87,C82), C73(C70,C51,C29,C37,C76),
 C88(C85,C74,C83,C90,C92), C48A(C49A,C52A,C66A,C79A,C62A), C90A(C92A,C88A,C85A,
 C74A,C83A), C86A(C78A,C47A,C40A,C89A,C91A)
4.f Tetrahedral OH refined with riding coordinates:
 O44(H44), O45(H45), O47(H47B), O45A(H45C), O46A(H46C)
4.g Idealised Me refined as rotating group:
 C81(H81A,H81B,H81C), C18(H18A,H18B,H18C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 134 electrons were 
found in a volume of 720\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
4[CH4O] per Asymmetric Unit 
which account for 144 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              77363
_shelx_fab_checksum              38098
_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 1.072
_oxdiff_exptl_absorpt_empirical_full_min 0.944