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_1564702
_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         'C36 H84 Cl4 In12 N8 O26, 2(Cl)'
_chemical_formula_sum            'C36 H84 Cl6 In12 N8 O26'
_chemical_formula_weight         2635.65
_chemical_name_systematic        InOC-1
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 90.1940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.05120(10)
_cell_length_b                   11.42060(10)
_cell_length_c                   20.21170(10)
_cell_measurement_reflns_used    38558
_cell_measurement_temperature    297.99(16)
_cell_measurement_theta_max      64.0050
_cell_measurement_theta_min      3.7910
_cell_volume                     3705.07(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.99(16)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_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    -15.00  73.00   0.50    0.05    --   -0.94  38.00 -30.00  176
  2  \w    -74.00  14.00   0.50    0.05    --   -0.94 -38.00  60.00  176
  3  \w    -17.00  72.00   0.50    0.05    --   -0.94  57.00-150.00  178
  4  \w      8.00 106.00   0.50    0.05    --   80.41 -99.00  30.00  196
  5  \w     20.00 111.00   0.50    0.05    --   80.41-125.00-180.00  182
  6  \w      8.00 104.00   0.50    0.05    --   80.41 -77.00-180.00  192
  7  \w      8.00 106.00   0.50    0.05    --   80.41 -99.00-180.00  196
  8  \w      8.00  66.00   0.50    0.05    --   80.41 -57.00  60.00  116
  9  \w     20.00 111.00   0.50    0.05    --   80.41-125.00  30.00  182
 10  \w      7.00  43.00   0.50    0.05    --   80.41 -38.00 -60.00   72
 11  \w     20.00 111.00   0.50    0.05    --   80.41-125.00 -60.00  182
 12  \w    -66.00  -9.00   0.50    0.05    --  -82.29  57.00   0.00  114
 13  \w   -156.00 -68.00   0.50    0.05    --  -82.29 -38.00 -90.00  176
 14  \w    -66.00  -9.00   0.50    0.05    --  -82.29  57.00  30.00  114
 15  \w    -43.00  -9.00   0.50    0.05    --  -82.29  38.00 -30.00   68
 16  \w    -66.00  -9.00   0.50    0.05    --  -82.29  57.00  60.00  114
 17  \w   -156.00 -68.00   0.50    0.05    --  -82.29 -38.00-120.00  176
 18  \w    -43.00  -9.00   0.50    0.05    --  -82.29  38.00-150.00   68
 19  \w    -43.00  -9.00   0.50    0.05    --  -82.29  38.00 150.00   68
 20  \w   -111.00 -20.00   0.50    0.05    --  -82.29 125.00  60.00  182
 21  \w    -43.00  -9.00   0.50    0.05    --  -82.29  38.00-120.00   68
 22  \w    -43.00  -9.00   0.50    0.05    --  -82.29  38.00-180.00   68
 23  \w   -155.00 -66.00   0.50    0.05    --  -82.29 -57.00  60.00  178
 24  \w   -111.00 -20.00   0.50    0.05    --  -82.29 125.00 -90.00  182
 25  \w    -16.00  75.00   0.50    0.05    --   -0.94  19.00 -60.00  182
 26  \w    -16.00  75.00   0.50    0.05    --   -0.94  19.00 120.00  182
 27  \w    -73.00  15.00   0.50    0.05    --   -0.94 -57.00   0.00  176
 28  \w    -24.00  72.00   0.50    0.05    --   -0.94  77.00 150.00  192
 29  \w   -156.00 -68.00   0.50    0.05    --  -82.29 -38.00   0.00  176
 30  \w   -156.00 -68.00   0.50    0.05    --  -82.29 -38.00  90.00  176
 31  \w   -156.00 -68.00   0.50    0.05    --  -82.29 -38.00 150.00  176
 32  \w   -155.00-126.00   0.50    0.05    --  -82.29 -57.00-150.00   58
;
_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      0.0418250000
_diffrn_orient_matrix_UB_12      -0.0908042000
_diffrn_orient_matrix_UB_13      0.0256141000
_diffrn_orient_matrix_UB_21      -0.0240010000
_diffrn_orient_matrix_UB_22      0.0316553000
_diffrn_orient_matrix_UB_23      0.0608306000
_diffrn_orient_matrix_UB_31      -0.0681228000
_diffrn_orient_matrix_UB_32      -0.0669659000
_diffrn_orient_matrix_UB_33      -0.0060433000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            43834
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         64.142
_diffrn_reflns_theta_min         3.803
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    21.288
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            light
_exptl_crystal_colour_modifier   light
_exptl_crystal_density_diffrn    2.362
_exptl_crystal_description       block
_exptl_crystal_F_000             2508
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.6
_refine_diff_density_max         1.128
_refine_diff_density_min         -1.335
_refine_diff_density_rms         0.174
_refine_ls_abs_structure_details
;
 Flack x determined using 3964 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         9088
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0595P)^2^+8.9904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0915
_reflns_Friedel_coverage         0.865
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                8895
_reflns_number_total             9088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04491e2.cif
_cod_data_source_block           InOC-1
_cod_database_code               1564702
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         In12CHONCl
_shelx_estimated_absorpt_t_max   0.028
_shelx_estimated_absorpt_t_min   0.021
_diffrn_oxdiff_digest_frames
;
01315327b64b33652a1d32372b9f7deff10474266a6
;
_diffrn_oxdiff_digest_hkl
;
01e81091a91d4acab5403871708933a4397708
;
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Others
 Fixed U12: O5(0) O11(0)
 Fixed U23: O5(0) O11(0)
 Fixed Uiso: H1(0.053) H2(0.049) H3(0.044) H4(0.05) H1A(0.071) H1B(0.071)
 H2A(0.06) H2B(0.06) H3A(0.045) H3B(0.045) H4A(0.081) H4B(0.081) H5A(0.062)
 H5B(0.062) H6A(0.051) H6B(0.051) H7A(0.048) H7B(0.048) H8A(0.054) H8B(0.054)
 H9A(0.045) H9B(0.045) H10A(0.068) H10B(0.068) H11A(0.058) H11B(0.058)
 H12A(0.089) H12B(0.089) H12C(0.089) H13A(0.057) H13B(0.057) H14A(0.066)
 H14B(0.066) H15A(0.071) H15B(0.071) H16A(0.065) H16B(0.065) H17A(0.069)
 H17B(0.069) H18A(0.093) H18B(0.093) H18C(0.093)
 Fixed X: O5(0.5) O11(0.5) H1(0.43115) H2(0.13273) H3(0.098789) H4(0.505382)
 H1A(0.469381) H1B(0.470138) H2A(0.307497) H2B(0.322064) H3A(0.351929)
 H3B(0.269919) H4A(0.295354) H4B(0.332628) H5A(0.202791) H5B(0.170891)
 H6A(0.101569) H6B(0.080145) H7A(0.054817) H7B(0.146061) H8A(0.107292)
 H8B(0.162177) H9A(0.245999) H9B(0.221895) H10A(0.185358) H10B(0.208023)
 H11A(0.344538) H11B(0.323997) H12A(0.316303) H12B(0.224576) H12C(0.258678)
 H13A(0.430851) H13B(0.340836) H14A(0.38242) H14B(0.433023) H15A(0.573457)
 H15B(0.625611) H16A(0.662866) H16B(0.570138) H17A(0.413009) H17B(0.392511)
 H18A(0.564166) H18B(0.473303) H18C(0.489778)
 Fixed Y: H1(0.385631) H2(0.773941) H3(0.599925) H4(0.215388) H1A(0.615148)
 H1B(0.558249) H2A(0.413043) H2B(0.525804) H3A(0.63556) H3B(0.566802)
 H4A(0.831833) H4B(0.88106) H5A(0.928165) H5B(0.816651) H6A(0.408479)
 H6B(0.538648) H7A(0.421469) H7B(0.371667) H8A(0.465313) H8B(0.578006)
 H9A(0.421915) H9B(0.354483) H10A(0.82466) H10B(0.934923) H11A(0.872992)
 H11B(0.865506) H12A(0.119242) H12B(0.15937) H12C(0.157883) H13A(0.114624)
 H13B(0.145352) H14A(0.168762) H14B(0.059011) H15A(0.058822) H15B(0.16818)
 H16A(0.133462) H16B(0.116783) H17A(0.446935) H17B(0.578773) H18A(0.835014)
 H18B(0.835284) H18C(0.877215)
 Fixed Z: O5(0.5) O11(0.5) H1(0.180931) H2(0.504372) H3(0.558247) H4(0.789358)
 H1A(0.213793) H1B(0.143049) H2A(0.226518) H2B(0.183808) H3A(0.27515)
 H3B(0.291749) H4A(0.366577) H4B(0.432716) H5A(0.443731) H5B(0.406369)
 H6A(0.41979) H6B(0.438338) H7A(0.529692) H7B(0.52705) H8A(0.646383)
 H8B(0.655482) H9A(0.683339) H9B(0.618199) H10A(0.600028) H10B(0.557395)
 H11A(0.545794) H11B(0.621581) H12A(0.488233) H12B(0.474004) H12C(0.546772)
 H13A(0.623747) H13B(0.64842) H14A(0.752581) H14B(0.729364) H15A(0.730201)
 H15B(0.751989) H16A(0.647616) H16B(0.624543) H17A(0.829714) H17B(0.814207)
 H18A(0.691018) H18B(0.719218) H18C(0.646575)
;
_shelx_res_checksum              42847
_shelx_hkl_checksum              16844
_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 2.931
_oxdiff_exptl_absorpt_empirical_full_min 0.454