pH-dependent formation of three porous In(III)-MOFs: framework diversity and selective gas adsorption
Zhang, Chengcheng; Qin, Yuanyuan; Duan, Lijuan; Wang, Lu; Wu, Yuewei; Guo, Yan; Song, Weiming; Liu, Xiangyu; Dalton Transactions  (2022) –; doi:10.1039/D1DT02935E

data_7709047
_publ_section_title
;
 pH-dependent formation of three porous In(III)-MOFs: framework diversity
 and selective gas adsorption
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02935E
_journal_year                    2022
_chemical_formula_moiety         'C52 H30 In3 N4 O18'
_chemical_formula_sum            'C52 H30 In3 N4 O18'
_chemical_formula_weight         1343.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-04 deposited with the CCDC.	2021-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.9446(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2038(2)
_cell_length_b                   22.6496(3)
_cell_length_c                   22.0902(3)
_cell_measurement_reflns_used    6731
_cell_measurement_temperature    156(10)
_cell_measurement_theta_max      73.3780
_cell_measurement_theta_min      4.2230
_cell_volume                     7194.93(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      156(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    -92.00  -4.00   1.00    1.50    --  -40.08 125.00 -90.00   88
  2  \w    -65.00  32.00   1.00    1.50    --  -40.08  38.00 -90.00   97
  3  \w     32.00 117.00   1.00    2.96    --  105.48-125.00  30.00   85
  4  \w     57.00 111.00   1.00    2.96    --  105.48-125.00-120.00   54
  5  \w     29.00 125.00   1.00    2.96    --  105.48 -30.00  30.00   96
  6  \w     45.00  95.00   1.00    2.96    --  105.48 -77.00  30.00   50
;
_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      -0.0106860000
_diffrn_orient_matrix_UB_12      0.0013962000
_diffrn_orient_matrix_UB_13      0.0669830000
_diffrn_orient_matrix_UB_21      -0.0040177000
_diffrn_orient_matrix_UB_22      0.0679836000
_diffrn_orient_matrix_UB_23      -0.0025475000
_diffrn_orient_matrix_UB_31      -0.1065095000
_diffrn_orient_matrix_UB_32      -0.0028524000
_diffrn_orient_matrix_UB_33      -0.0308124000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24333
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         3.641
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.109
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       block
_exptl_crystal_F_000             2644
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         3.256
_refine_diff_density_min         -1.392
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     997
_refine_ls_number_reflns         12626
_refine_ls_number_restraints     3569
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0699
_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^)+(0.0963P)^2^+58.7921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1928
_refine_ls_wR_factor_ref         0.2051
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9769
_reflns_number_total             12626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02935e2.cif
_cod_data_source_block           dl-4
_cod_original_cell_volume        7194.95(19)
_cod_database_code               7709047
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     C4A-C4-MGCL2
_shelx_estimated_absorpt_t_max   0.339
_shelx_estimated_absorpt_t_min   0.308
_reflns_odcompleteness_completeness 88.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
2. Rigid bond restraints
 O7, C18, O3A, O8, C24A, C6AA, C17, C20, C22A, C25A, C21, C21A, C19, C26A,
 C27A, C28A, N4A, C29A, C30A, C22, N4, C25, C23, C26, C24, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6A, C5A, C7A, C8A, C9A, C10A, O7A, O11, O6A, C11A, C31, C30, C28, C34, C33,
 C29, C16A, C12A, C13A, C14A, N3A, C15A, C32, O12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6A, C5A, C7A, C8A, C9A, C10A, O7A, O11, O6A, C11A, C31, C30, C28, C34, C33,
 C29, C16A, C12A, C13A, C14A, N3A, C15A, C32, O12, C37, C36, N3, C38, C39, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C15 \\sim C18 \\sim C16 \\sim C24A \\sim C17 \\sim C20 \\sim C22A \\sim C25A
\\sim C21: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C26A \\sim C27A \\sim C28A \\sim N4A \\sim C29A \\sim C30A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
O7 \\sim C18 \\sim O3A \\sim O8 \\sim C24A \\sim C6AA \\sim C17 \\sim C20 \\sim
C22A \\sim C25A \\sim C21 \\sim C21A \\sim C19 \\sim C26A \\sim C27A \\sim C28A
\\sim N4A \\sim C29A \\sim C30A \\sim C22 \\sim N4 \\sim C25 \\sim C23 \\sim
C26 \\sim C24 \\sim C16: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C6A \\sim C5A \\sim C7A \\sim C8A \\sim C9A \\sim C10A \\sim O7A \\sim O11
\\sim O6A \\sim C11A \\sim C31 \\sim C30 \\sim C28 \\sim C34 \\sim C33 \\sim
C29 \\sim C16A \\sim C12A \\sim C13A \\sim C14A \\sim N3A \\sim C15A \\sim C32
\\sim O12: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C6A \\sim C5A \\sim C7A \\sim C8A \\sim C9A \\sim C10A \\sim O7A \\sim O11
\\sim O6A \\sim C11A \\sim C31 \\sim C30 \\sim C28 \\sim C34 \\sim C33 \\sim
C29 \\sim C16A \\sim C12A \\sim C13A \\sim C14A \\sim N3A \\sim C15A \\sim C32
\\sim O12 \\sim C37 \\sim C36 \\sim N3 \\sim C38 \\sim C39 \\sim C35: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C6 \\sim C47 \\sim C9 \\sim C7 \\sim C8 \\sim C44 \\sim C5 \\sim C15 \\sim C45
\\sim C2 \\sim C41 \\sim C3 \\sim C48 \\sim C46 \\sim C1 \\sim C42 \\sim C4
\\sim C40 \\sim C2A \\sim C43 \\sim C3A \\sim C18A \\sim C19A \\sim C4A \\sim
C17A \\sim C1A \\sim C12 \\sim C20A \\sim C10 \\sim C11 \\sim C49 \\sim C13
\\sim C51 \\sim C52 \\sim C50 \\sim C27 \\sim C6A \\sim C5A \\sim C7A \\sim C8A
\\sim C9A \\sim C10A \\sim C14 \\sim C18 \\sim C16 \\sim C11A \\sim C24A \\sim
C6AA \\sim C17 \\sim C20 \\sim C22A \\sim C25A \\sim C21 \\sim C21A \\sim C19
\\sim C26A \\sim C27A \\sim C28A \\sim C29A \\sim C30A \\sim C31 \\sim C30
\\sim C28 \\sim C34 \\sim C33 \\sim C29 \\sim C16A \\sim C12A \\sim C13A \\sim
C14A \\sim C15A \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C32
\\sim C37 \\sim C36 \\sim C35 \\sim C39 \\sim C38 \\sim N1 \\sim N2 \\sim N4A
\\sim N3A \\sim N4 \\sim N3: within 3.8A with sigma of 0.03 and sigma for
terminal atoms of 0.06
Uanis(O7) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(C24A) \\sim Ueq,
Uanis(C6AA) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C22A)
\\sim Ueq, Uanis(C25A) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C21A) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C26A) \\sim Ueq, Uanis(C27A) \\sim Ueq, Uanis(C28A)
\\sim Ueq, Uanis(N4A) \\sim Ueq, Uanis(C29A) \\sim Ueq, Uanis(C30A) \\sim Ueq,
Uanis(C22) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O5A) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O4A)
\\sim Ueq, Uanis(O6A) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq,
Uanis(O7A) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(O1)
\\sim Ueq, Uanis(O2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C17A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O13(0.5) O1(0.5) C2A(0.5) H2A(0.5) O5A(0.5) C3A(0.5) H3A(0.5)
 C18A(0.5) H18A(0.5) C19A(0.5) H19A(0.5) C4A(0.5) H4A(0.5) C17A(0.5) H17A(0.5)
 C1A(0.5) H1A(0.5) O2(0.5) C12(0.5) H12(0.5) O2A(0.5) C20A(0.5) H20A(0.5)
 C10(0.5) H10(0.5) C11(0.5) H11(0.5) C49(0.5) H49(0.5) C13(0.5) H13(0.5)
 O14(0.5) O4A(0.5) C51(0.5) H51(0.5) C52(0.5) H52(0.5) C50(0.5) H50(0.5)
 O1A(0.5) C6A(0.5) H6A(0.5) C5A(0.5) C7A(0.5) H7A(0.5) C8A(0.5) C9A(0.5)
 H9A(0.5) C10A(0.5) C18(0.5) H16A(0.5) H16(0.5) O3A(0.5) O8(0.5) O7A(0.5)
 O11(0.5) O6A(0.5) C11A(0.5) C24A(0.5) C6AA(0.5) C17(0.5) H17B(0.5) C20(0.5)
 H20(0.5) C22A(0.5) C25A(0.5) H25A(0.5) C21(0.5) C21A(0.5) H21A(0.5) C19(0.5)
 C26A(0.5) C27A(0.5) H27A(0.5) C28A(0.5) H28A(0.5) N4A(0.5) C29A(0.5) H29A(0.5)
 C30A(0.5) H30A(0.5) C31(0.5) C30(0.5) H30(0.5) C28(0.5) C34(0.5) H34(0.5)
 C33(0.5) C29(0.5) H29(0.5) C16A(0.5) H16B(0.5) C12A(0.5) C13A(0.5) H13A(0.5)
 C14A(0.5) H14A(0.5) N3A(0.5) C15A(0.5) H15A(0.5) C22(0.5) C23(0.5) H23(0.5)
 C24(0.5) H24(0.5) N4(0.5) C25(0.5) H25(0.5) C26(0.5) H26(0.5) C32(0.5)
 O12(0.5) N3(0.5) C37(0.5) H37(0.5) C36(0.5) H36(0.5) C35(0.5) C39(0.5)
 H39(0.5) C38(0.5) H38(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 O18(H18), O17(H17), C7(H7), C45(H45), C3(H3), C42(H42), C4(H4), C2A(H2A),
 C43(H43), C3A(H3A), C18A(H18A), C19A(H19A), C4A(H4A), C17A(H17A), C1A(H1A),
 C12(H12), C20A(H20A), C10(H10), C11(H11), C49(H49), C13(H13), C51(H51),
 C52(H52), C50(H50), C6A(H6A), C7A(H7A), C9A(H9A), C16(H16A), C16(H16),
 C17(H17B), C20(H20), C25A(H25A), C21A(H21A), C27A(H27A), C28A(H28A),
 C29A(H29A), C30A(H30A), C30(H30), C34(H34), C29(H29), C16A(H16B), C13A(H13A),
 C14A(H14A), C15A(H15A), C23(H23), C24(H24), C25(H25), C26(H26), C37(H37),
 C36(H36), C39(H39), C38(H38)
5.b Fitted hexagon refined as free rotating group:
 C26A(C27A,C28A,N4A,C29A,C30A), C16A(C12A,C13A,C14A,N3A,C15A), C22(C23,C24,N4,
 C25,C26), N3(C37,C36,C35,C39,C38)
;
_shelx_res_checksum              79461
_shelx_fab_checksum              47545
_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 1.407
_oxdiff_exptl_absorpt_empirical_full_min 0.712