A highly robust cluster-based indium(III)-organic framework with efficient catalytic activity in cycloaddition of CO<sub>2</sub> and Knoevenagel condensation.
Lv, Hongxiao; Fan, Liming; Hu, Tuoping; Jiao, Chenxu; Zhang, Xiutang; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d2dt04043c

data_7712393
_publ_section_title
;
 A highly robust cluster-based indium(III)-organic framework with
 efficient catalytic activity in cycloaddition of CO<sub>2</sub> and
 Knoevenagel condensation.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt04043c
_journal_year                    2023
_chemical_formula_moiety         '0.17(C348 H162 In24 N12 O156)'
_chemical_formula_sum            'C58 H27 In4 N2 O26'
_chemical_formula_weight         1627.09
_space_group_crystal_system      hexagonal
_space_group_IT_number           193
_space_group_name_Hall           '-P 6c 2'
_space_group_name_H-M_alt        'P 63/m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2d8zk7
_audit_creation_date             2022-10-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-10-15 deposited with the CCDC.	2023-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   22.1330(2)
_cell_length_b                   22.1330(2)
_cell_length_c                   38.3955(3)
_cell_measurement_reflns_used    26293
_cell_measurement_temperature    298
_cell_measurement_theta_max      76.3340
_cell_measurement_theta_min      3.2180
_cell_volume                     16288.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.0
_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 0.998
_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     95.00 173.00   1.00    2.20    --  106.49 125.00  30.00   78
  2  \w    103.00 178.00   1.00    2.20    --  106.49 111.00  64.00   75
  3  \w    105.00 178.00   1.00    2.20    --  106.49 108.00 170.00   73
  4  \w   -155.00 -75.00   1.00    2.20    --  -86.25-122.00 -42.00   80
  5  \w    -33.00  27.00   1.00    0.30    --  -48.45  27.00 -26.00   60
  6  \w    -27.00  27.00   1.00    0.30    --  -48.45  19.00 120.00   54
  7  \w     34.00 104.00   1.00    2.20    --  106.49 -77.00   0.00   70
  8  \w     40.00  66.00   1.00    2.20    --  106.49 -57.00 -60.00   26
  9  \w     38.00  64.00   1.00    2.20    --  106.49 -57.00-150.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0392345000
_diffrn_orient_matrix_UB_12      0.0798202000
_diffrn_orient_matrix_UB_13      -0.0047561000
_diffrn_orient_matrix_UB_21      0.0644668000
_diffrn_orient_matrix_UB_22      -0.0024217000
_diffrn_orient_matrix_UB_23      -0.0131752000
_diffrn_orient_matrix_UB_31      -0.0275651000
_diffrn_orient_matrix_UB_32      -0.0092955000
_diffrn_orient_matrix_UB_33      -0.0376115000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            56392
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.063
_diffrn_reflns_theta_max         67.063
_diffrn_reflns_theta_min         3.258
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.127
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.995
_exptl_crystal_description       block
_exptl_crystal_F_000             4758
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.056
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.097
_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     270
_refine_ls_number_reflns         5172
_refine_ls_number_restraints     163
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0643P)^2^+76.6842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1438
_refine_ls_wR_factor_ref         0.1452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4898
_reflns_number_total             5172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04043c2.cif
_cod_data_source_block           0329a30
_cod_original_cell_volume        16288.8(3)
_cod_database_code               7712393
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         EuCNO
_shelx_estimated_absorpt_t_max   0.674
_shelx_estimated_absorpt_t_min   0.291
_diffrn_oxdiff_digest_frames
;
015a41a34abf3e983e7bc42b4ea465fb20005422d45
;
_diffrn_oxdiff_digest_hkl
;
01d2410a38173b1961f282ee48be2371df886b
;
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 C13-C14 = C16-C17 = C17-C18
 1.37 with sigma of 0.02
 C13-C18
 1.38 with sigma of 0.02
 C14-C15 = C15-C16
 1.36 with sigma of 0.02
 C19-O2
 1.22 with sigma of 0.02
 C19-C20
 1.36 with sigma of 0.02
 C13-C17
 2.38 with sigma of 0.04
 C14-C16
 2.36 with sigma of 0.04
 C13-C15 = C15-C17 = C16-C18
 2.37 with sigma of 0.04
 C13-C14 \\sim C14-C15 \\sim C15-C16 \\sim C16-C17 \\sim C17-C18 \\sim C18-C13
 with sigma of 0.02
 C13-C17 \\sim C13-C15 \\sim C17-C15 \\sim C16-C14 \\sim C16-C18 \\sim C18-C14
 with sigma of 0.04
2. Restrained planarity
 C13, C14, C15, C16, C17, C18
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C9 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim O3 \\sim
O7: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
within 1.7A
C19 \\sim O2 \\sim C20: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.004 within 1.7A
Uanis(O1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.001
4. Rigid body (RIGU) restrains
 C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, O2, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O7)=1-FVAR(1)
 Sof(O3)=FVAR(1)
 Fixed Sof: C13(0.5) C14(0.5) H14(0.5) C15(0.5) H15(0.5) C16(0.25) C17(0.5)
 H17(0.5) C18(0.5) H18(0.5) C19(0.25) O2(0.5) C20(0.25) H20A(0.25) H20B(0.25)
 H20C(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C10(H10), C11(H11), C14(H14), C15(H15), C17(H17), C18(H18)
6.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              67077
_shelx_fab_checksum              30011
_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 1.994
_oxdiff_exptl_absorpt_empirical_full_min 0.627