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_7709048
_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      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-06
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2021-11-08 deposited with the CCDC.	2021-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 124.201(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.8733(11)
_cell_length_b                   20.7854(8)
_cell_length_c                   22.4567(9)
_cell_measurement_reflns_used    4801
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      51.260
_cell_measurement_theta_min      2.583
_cell_volume                     10374.5(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      193.00
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'BRUKER D8 VENTURE PHOTON II'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17852
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.179
_diffrn_reflns_theta_min         2.532
_exptl_absorpt_coefficient_mu    2.641
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.824
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.476
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         17852
_refine_ls_number_restraints     478
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0746
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1478P)^2^+7.3594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2224
_refine_ls_wR_factor_ref         0.2449
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12038
_reflns_number_total             17852
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02935e2.cif
_cod_data_source_block           znz6736_0m_5_sq
_cod_original_cell_volume        10374.5(7)
_cod_database_code               7709048
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.742
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4344(14)
 0.5656(14)
2. 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
3. Restrained distances
 C18-C21
 1.51 with sigma of 0.001
 C26-N3 = N3-C26_$1
 1.47 with sigma of 0.02
 C28-N4 = N4-C29
 1.47 with sigma of 0.02
 C26-N3 = N3-C27
 1.47 with sigma of 0.02
 C26-C26_$1
 2.401 with sigma of 0.04
 C26-C27
 2.401 with sigma of 0.04
 C28-C29
 2.401 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(C26) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N3, C26, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Same fragment restrains
{C19, C22A, C23A, C24A, N2A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C19, C22, C23, C24, N2, C25, C30}
7. Others
 Sof(C22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(N2A)=Sof(C25A)=
 Sof(H25A)=Sof(C26A)=Sof(H26A)=1-FVAR(1)
 Sof(C22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(N2)=Sof(C25)=Sof(H25)=
 Sof(C30)=Sof(H30)=FVAR(1)
 Fixed Sof: N3(0.5) H3A(0.5) H3B(0.5) C26(0.5) H26B(0.5) H26C(0.5) H26D(0.5)
 C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) N4(0.5) H4A(0.5) H4B(0.5) C29(0.5)
 H29A(0.5) H29B(0.5) H29C(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5)
8.a Riding coordinates:
 C26(H26B,H26C,H26D), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C)
8.b Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B)
8.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13), C16(H16),
 C17(H17), C20(H20), C23(H23), C24(H24), C25(H25), C30(H30), C23A(H23A),
 C24A(H24A), C25A(H25A), C26A(H26A)
8.d Fitted hexagon refined as free rotating group:
 C22(C23,C24,N2,C25,C30)
8.e Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C)
;
_shelx_res_checksum              57543
_shelx_fab_checksum              316
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'