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_1564704
_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 H72 Br4 In12 N12 O34, Br2'
_chemical_formula_sum            'C56 H68 Br6 In12 N12 O34'
_chemical_formula_weight         3310.52
_chemical_name_systematic        InOC-4
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-01-24
_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                   16.1018(4)
_cell_length_b                   16.1018(4)
_cell_length_c                   20.4257(8)
_cell_measurement_reflns_used    4191
_cell_measurement_temperature    100.01(12)
_cell_measurement_theta_max      74.2080
_cell_measurement_theta_min      3.3990
_cell_volume                     5295.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.01(12)
_diffrn_detector_area_resol_mean 10.3468
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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      0.00 121.00   1.00    1.50    --   41.41  19.00   0.00  121
  2  \w    104.00 178.00   1.00    3.00    --  108.23 111.00 120.00   74
  3  \w    103.00 178.00   1.00    3.00    --  108.23  77.00-120.00   75
  4  \w    104.00 178.00   1.00    3.00    --  108.23 111.00-120.00   74
  5  \w     82.00 178.00   1.00    3.00    --  108.23  45.00-150.00   96
  6  \w     17.00  63.00   1.00    1.50    --   41.41  38.00 120.00   46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7312
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        66.582
_diffrn_reflns_theta_max         66.582
_diffrn_reflns_theta_min         3.495
_exptl_absorpt_coefficient_mu    23.728
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    2.076
_exptl_crystal_description       block
_exptl_crystal_F_000             3116
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.712
_refine_diff_density_min         -2.140
_refine_diff_density_rms         0.291
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4325
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1519P)^2^+83.3473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1999
_refine_ls_wR_factor_ref         0.2069
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_full    0.844
_reflns_Friedel_fraction_max     0.844
_reflns_number_gt                4108
_reflns_number_total             4325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04491e2.cif
_cod_data_source_block           InOC-4
_cod_database_code               1564704
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.330
_shelx_estimated_absorpt_t_min   0.163
_olex2_refinement_description
;
1. Others
 Fixed Sof: Br2(0.5)
 Fixed U13: O5(0)
 Fixed U23: O5(0)
 Fixed Uiso: H2(0.061) H1(0.072) H2A(0.071) H3(0.067) H5(0.094) H6(0.079)
 H9A(0.064) H9B(0.064) H10A(0.063) H10B(0.063) H11A(0.075) H11B(0.075)
 H12A(0.099) H12B(0.099) H13A(0.046) H13B(0.046) H14A(0.06) H14B(0.06)
 Fixed X: O5(0.5) H2(0.149709) H1(0.103788) H2A(0.368003) H3(0.323131)
 H5(0.10551) H6(0.154146) H9A(0.082368) H9B(0.139736) H10A(0.195157)
 H10B(0.206809) H11A(0.260938) H11B(0.199844) H12A(0.356978) H12B(0.295813)
 H13A(0.317532) H13B(0.352543) H14A(0.223309) H14B(0.184085)
 Fixed Y: O5(0.5) H2(0.457623) H1(0.512638) H2A(0.524177) H3(0.520814)
 H5(0.414917) H6(0.417364) H9A(0.616112) H9B(0.64395) H10A(0.598067)
 H10B(0.685853) H11A(0.414926) H11B(0.354432) H12A(0.349793) H12B(0.300012)
 H13A(0.634046) H13B(0.543348) H14A(0.540013) H14B(0.58655)
 Fixed Z: H2(0.667508) H1(0.572869) H2A(0.285078) H3(0.176024) H5(0.239286)
 H6(0.343136) H9A(0.490236) H9B(0.548332) H10A(0.421687) H10B(0.45441)
 H11A(0.7522) H11B(0.716189) H12A(0.709513) H12B(0.665231) H13A(0.702716)
 H13B(0.705796) H14A(0.751849) H14B(0.691714)
;
_shelx_res_checksum              52929
_shelx_hkl_checksum              51524
_shelx_fab_checksum              5299
_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
;