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_7709049
_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         'C26 H14 In N2 O8, C2 H8 N'
_chemical_formula_sum            'C28 H22 In N3 O8'
_chemical_formula_weight         643.30
_space_group_crystal_system      tetragonal
_space_group_IT_number           135
_space_group_name_Hall           '-P 4c 2ab'
_space_group_name_H-M_alt        'P 42/m b c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-11-08 deposited with the CCDC.	2021-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.2125(7)
_cell_length_b                   20.2125(7)
_cell_length_c                   22.9119(9)
_cell_measurement_reflns_used    9661
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      56.843
_cell_measurement_theta_min      3.805
_cell_volume                     9360.5(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      192.99
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-III CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            173822
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.297
_diffrn_reflns_theta_min         3.805
_diffrn_source_current           2.86
_diffrn_source_power             0.1993706
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.883
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.5732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1099 before and 0.0796 after correction.
The Ratio of minimum to maximum transmission is 0.7630.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.913
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.136
_refine_diff_density_min         -1.608
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4939
_refine_ls_number_restraints     529
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1013P)^2^+20.1330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.1812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4470
_reflns_number_total             4939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02935e2.cif
_cod_data_source_block           1_c
_cod_original_cell_volume        9360.5(7)
_cod_database_code               7709049
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C23-C24
 2.2 with sigma of 0.01
 N2-C23 = N2-C24
 1.45 with sigma of 0.01
 C8_2-C7_2
 1.5 with sigma of 0.01
 N2-C23 \\sim N2-C24
 with sigma of 0.01
3. Restrained planarity
 C8_2, C9_2, C10_2, N1_2, C11_2, C12_2, C7_2
 with sigma of 0.01
 C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2.5A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 2.5A
Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq: with sigma of 0.006 and sigma for terminal atoms of 0.012
5. Others
 Fixed Sof: C10(0.5) H10(0.5) C11(0.5) H11(0.5) C12(0.5) H12(0.5) C13(0.5)
 H13(0.5) N2(0.5) H2A(0.5) H2B(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
 C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C1(0.5) C13(0.5) C2(0.5) C3(0.5)
 H3(0.5) C4(0.5) H4(0.5) C5(0.5) C6(0.5) H6(0.5) C7(0.5) C8(0.5) C9(0.5)
 H9(0.5) C10(0.5) H10(0.5) N1(0.5) C11(0.5) H11(0.5) C12(0.5) H12(0.5) O2(0.5)
 O1(0.5)
 Fixed Y: C23(0.497489) C24(0.42077)
6.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B)
6.b Me refined with riding coordinates:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
6.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C3(H3), C6(H6), C7(H7), C3(H3),
 C4(H4), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12)
6.d Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7), C8(C9,C10,N1,C11,C12)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              52944
_shelx_fab_checksum              87365
_olex2_submission_special_instructions 'No special instructions were received'