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_1564703
_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 F4 In12 N8 O26, 2(Cl)'
_chemical_formula_sum            'C56 H88 Cl6 F4 In12 N8 O26'
_chemical_formula_weight         2955.88
_chemical_name_systematic        InOC-5
_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                   15.9744(2)
_cell_length_b                   15.9744(2)
_cell_length_c                   19.4804(5)
_cell_measurement_reflns_used    8429
_cell_measurement_temperature    100.03(19)
_cell_measurement_theta_max      74.5180
_cell_measurement_theta_min      3.8890
_cell_volume                     4971.04(16)
_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      100.03(19)
_diffrn_detector_area_resol_mean 5.1734
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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      6.00  82.00   1.00    1.50    --   41.04 -99.00-180.00   76
  2  \w     27.00  97.00   1.00    1.50    --   41.04-125.00 150.00   70
  3  \w     27.00  97.00   1.00    1.50    --   41.04-125.00 -90.00   70
  4  \w     97.00 178.00   1.00    6.00    --  108.23 125.00  60.00   81
  5  \w     26.00 106.00   1.00    6.00    --  108.23 -94.00 -30.00   80
  6  \w    103.00 178.00   1.00    6.00    --  108.23 110.00 -49.00   75
  7  \w     82.00 178.00   1.00    6.00    --  108.23  45.00  30.00   96
  8  \w     13.00 114.00   1.00    1.50    --   41.04  57.00 150.00  101
  9  \w     13.00 114.00   1.00    1.50    --   41.04  57.00 -60.00  101
 10  \w     80.00 174.00   1.00    6.00    --  108.23  30.00-150.00   94
;
_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     1.54178
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10192
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        58.930
_diffrn_reflns_theta_max         58.930
_diffrn_reflns_theta_min         3.913
_exptl_absorpt_coefficient_mu    23.891
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41355
_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            'clear light'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_density_diffrn    1.975
_exptl_crystal_description       block
_exptl_crystal_F_000             2828
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.480
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Flack x determined using 1540 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.028(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3465
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0358P)^2^+32.2449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    0.938
_reflns_Friedel_fraction_max     0.938
_reflns_number_gt                3400
_reflns_number_total             3465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04491e2.cif
_cod_data_source_block           InOC-5
_cod_original_cell_volume        4971.04(18)
_cod_database_code               1564703
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.381
_shelx_estimated_absorpt_t_min   0.251
_olex2_refinement_description
;
1. Others
 Fixed U13: O2(0) Cl2(0)
 Fixed U23: O2(0) Cl2(0)
 Fixed Uiso: H00D(0.032) H00E(0.038) H2(0.084) H3(0.114) H5(0.091) H6(0.085)
 H7A(0.108) H7B(0.108) H8A(0.045) H8B(0.045) H9A(0.037) H9B(0.037) H10A(0.037)
 H10B(0.037) H11A(0.041) H11B(0.041) H12A(0.03) H12B(0.03) H13A(0.051)
 H13B(0.051) H14A(0.046) H14B(0.046)
 Fixed X: O2(0.5) H00D(0.861528) H00E(0.906939) H2(0.384913) H3(0.396746)
 H5(0.554031) H6(0.5345) H7A(0.654183) H7B(0.717286) H8A(0.744148)
 H8B(0.809099) H9A(0.793261) H9B(0.827578) H10A(0.692739) H10B(0.656361)
 H11A(0.866187) H11B(0.922067) H12A(0.804385) H12B(0.795765) H13A(0.948018)
 H13B(0.856084) H14A(0.901765) H14B(0.876905) Cl2(1)
 Fixed Y: O2(0.5) H00D(0.552584) H00E(0.496995) H2(0.830909) H3(0.890767)
 H5(0.714619) H6(0.639986) H7A(0.676348) H7B(0.71009) H8A(0.597464)
 H8B(0.657995) H9A(0.469439) H9B(0.420842) H10A(0.371618) H10B(0.46495)
 H11A(0.36473) H11B(0.387813) H12A(0.403011) H12B(0.314787) H13A(0.543508)
 H13B(0.532316) H14A(0.651545) H14B(0.672974) Cl2(0.5)
 Fixed Z: H00D(0.66756) H00E(0.566029) H2(0.674084) H3(0.782238) H5(0.832356)
 H6(0.729815) H7A(0.712045) H7B(0.654928) H8A(0.756688) H8B(0.719102)
 H9A(0.75962) H9B(0.693421) H10A(0.714124) H10B(0.718626) H11A(0.550458)
 H11B(0.484913) H12A(0.416542) H12B(0.455294) H13A(0.46156) H13B(0.4298)
 H14A(0.531622) H14B(0.453761)
;
_shelx_res_checksum              78414
_shelx_hkl_checksum              24953
_shelx_fab_checksum              82786
_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
;