Molecular Bixbyite-Like In12-Oxo Clusters with Tunable Functionalization Sites for Lithography Patterning Applications
Yi, Xiaofeng; Wang, Di; Li, Fan; Zhang, Jian; Zhang, Lei; Chemical Science  (2021) –; doi:10.1039/D1SC04491E

data_1564705
_publ_section_title
;
 Molecular Bixbyite-Like In12-Oxo Clusters with Tunable Functionalization
 Sites for Lithography Patterning Applications
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04491E
_journal_year                    2021
_chemical_formula_moiety         'C56 H88 Cl4 In12 N12 O34, Cl2'
_chemical_formula_sum            'C56 H88 Cl6 In12 N12 O34'
_chemical_formula_weight         3063.92
_chemical_name_systematic        InOC-3
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-19 deposited with the CCDC.	2021-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.9892(2)
_cell_length_b                   15.9892(2)
_cell_length_c                   20.3659(5)
_cell_measurement_reflns_used    10426
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      73.2190
_cell_measurement_theta_min      3.4470
_cell_volume                     5206.63(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3468
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_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    -67.00  31.00   1.00    1.25    --  -41.41  57.00  30.00   98
  2  \w    -86.00 -52.00   1.00    1.25    --  -41.41 125.00  90.00   34
  3  \w   -113.00 -18.00   1.00    1.25    --  -41.41 -57.00-120.00   95
  4  \w    -61.00  33.00   1.00    1.25    --  -41.41  38.00-180.00   94
  5  \w     28.00  53.00   1.00    1.25    --   41.41-125.00  90.00   25
  6  \w     28.00 131.00   1.00    2.50    --  104.65 -30.00-120.00  103
  7  \w     98.00 124.00   1.00    2.50    --  104.65 -77.00 -30.00   26
  8  \w     37.00 106.00   1.00    2.50    --  104.65 -94.00  30.00   69
  9  \w     80.00 106.00   1.00    2.50    --  104.65 -94.00-120.00   26
 10  \w     40.00 103.00   1.00    2.50    --  104.65 -94.00 120.00   63
 11  \w    123.00 178.00   1.00    2.50    --  104.65  77.00-180.00   55
 12  \w    118.00 163.00   1.00    2.50    --  104.65 125.00 -30.00   45
 13  \w    150.00 176.00   1.00    2.50    --  104.65 125.00  60.00   26
 14  \w     69.00 113.00   1.00    2.50    --  104.65-125.00  30.00   44
 15  \w    138.00 178.00   1.00    2.50    --  104.65  77.00-150.00   40
 16  \w     24.00 139.00   1.00    2.50    --  104.65 -15.00 120.00  115
 17  \w     36.00 106.00   1.00    2.50    --  104.65 -94.00-180.00   70
 18  \w     45.00  71.00   1.00    2.50    --  104.65 -45.00  90.00   26
 19  \w     30.00 106.00   1.00    2.50    --  104.65 -94.00 -90.00   76
 20  \w     72.00 148.00   1.00    2.50    --  104.65 -15.00   0.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0527043000
_diffrn_orient_matrix_UB_12      -0.0752792000
_diffrn_orient_matrix_UB_13      -0.0228467000
_diffrn_orient_matrix_UB_21      -0.0327697000
_diffrn_orient_matrix_UB_22      0.0118358000
_diffrn_orient_matrix_UB_23      -0.0705077000
_diffrn_orient_matrix_UB_31      0.0737638000
_diffrn_orient_matrix_UB_32      0.0589119000
_diffrn_orient_matrix_UB_33      -0.0150489000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19375
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.436
_diffrn_reflns_theta_min         3.514
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.853
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellowish
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_description       block
_exptl_crystal_F_000             2940
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.226
_refine_diff_density_min         -1.401
_refine_diff_density_rms         0.192
_refine_ls_abs_structure_details
;
 Flack x determined using 2179 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.033(13)
_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     276
_refine_ls_number_reflns         5146
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0721P)^2^+92.8556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.1484
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                4868
_reflns_number_total             5146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04491e2.cif
_cod_data_source_block           InOC-3
_cod_original_cell_volume        5206.63(18)
_cod_database_code               1564705
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         In
_shelx_estimated_absorpt_t_max   0.395
_shelx_estimated_absorpt_t_min   0.188
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Others
 Fixed Sof: Cl2(0.5)
 Fixed U13: O6(0)
 Fixed U23: O6(0)
 Fixed Uiso: H1(0.106) H2(0.084) H2A(0.091) H3(0.087) H5(0.142) H6(0.114)
 H7A(0.09) H7B(0.09) H8A(0.077) H8B(0.077) H9A(0.124) H9B(0.124) H10A(0.101)
 H10B(0.101) H11A(0.077) H11B(0.077) H12A(0.09) H12B(0.09) H13A(0.1) H13B(0.1)
 H14A(0.086) H14B(0.086)
 Fixed X: O6(0.5) H1(0.094579) H2(0.14536) H2A(0.473358) H3(0.474122)
 H5(0.591574) H6(0.589606) H7A(0.376179) H7B(0.355851) H8A(0.409461)
 H8B(0.318966) H9A(0.282733) H9B(0.348265) H10A(0.197611) H10B(0.264726)
 H11A(0.348494) H11B(0.315127) H12A(0.216093) H12B(0.180497) H13A(0.122622)
 H13B(0.100369) H14A(0.14187) H14B(0.052678)
 Fixed Y: O6(0.5) H1(0.493337) H2(0.546013) H2A(0.679682) H3(0.636304)
 H5(0.842993) H6(0.890896) H7A(0.918813) H7B(0.858857) H8A(0.807642)
 H8B(0.794677) H9A(0.704818) H9B(0.674631) H10A(0.651827) H10B(0.59403)
 H11A(0.460518) H11B(0.368316) H12A(0.459415) H12B(0.41429) H13A(0.67014)
 H13B(0.648666) H14A(0.532339) H14B(0.543834)
 Fixed Z: H1(0.567616) H2(0.666963) H2A(0.822335) H3(0.713745) H5(0.661086)
 H6(0.763705) H7A(0.509202) H7B(0.44999) H8A(0.574059) H8B(0.546164)
 H9A(0.65178) H9B(0.703606) H10A(0.716159) H10B(0.748808) H11A(0.707231)
 H11B(0.704547) H12A(0.750771) H12B(0.688214) H13A(0.46193) H13B(0.535151)
 H14A(0.438388) H14B(0.469355)
;
_shelx_res_checksum              35697
_shelx_hkl_checksum              67593
_shelx_fab_checksum              79734
_platon_squeeze_void_probe_radius 1.20
_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 1.914
_oxdiff_exptl_absorpt_empirical_full_min 0.584