A 2-fold interpenetrating 3D pillar-layered MOF for the gas separation and detection of metal ions.
Peng, Guoqiang; Su, Zhibo; Hu, Falu; Ji, Zhenyu; Di, Zhengyi; Li, Guihua; Gao, Tingting; Zhou, Guowei; Wu, Mingyan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16815–16820; doi:10.1039/d4dt02024c

data_7717127
_publ_section_title
;
 A 2-fold interpenetrating 3D pillar-layered MOF for the gas separation
 and detection of metal ions.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16815
_journal_page_last               16820
_journal_paper_doi               10.1039/d4dt02024c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C21.13 H10.40 F2 N1.13 O4 S0.37 Zn, 1[C3H7NO]'
_chemical_formula_sum            'C21.13 H10.4 F2 N1.13 O4 S0.37 Zn'
_chemical_formula_weight         459.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-08-31
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-09-05 deposited with the CCDC.	2024-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.472(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.8989(6)
_cell_length_b                   28.7314(10)
_cell_length_c                   10.1425(4)
_cell_measurement_reflns_used    6780
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      72.529
_cell_measurement_theta_min      3.204
_cell_volume                     4582.5(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15878
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.530
_diffrn_reflns_theta_min         3.076
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.169
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0935 before and 0.0615 after correction.
The Ratio of minimum to maximum transmission is 0.7902.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.170
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.113
_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     413
_refine_ls_number_reflns         4561
_refine_ls_number_restraints     509
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0701
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1350P)^2^+15.9412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2000
_refine_ls_wR_factor_ref         0.2190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3491
_reflns_number_total             4561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02024c2.cif
_cod_data_source_block           p
_cod_depositor_comments          'Adding full bibliography for 7717127.cif.'
_cod_original_formula_sum        'C21.13 H10.40 F2 N1.13 O4 S0.37 Zn'
_cod_database_code               7717127
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.796
_shelx_estimated_absorpt_t_min   0.766
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{S1, N2}
3. Restrained planarity
 C2, C3A, C4A, C5A, C6A, C7A, F1A, C8
 with sigma of 0.01
 C19, N1, C17A, C18A, C20A, C21A
 with sigma of 0.01
 C10, C13, C11A, C12A, C15A, C16A, F2A, C14, C9
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C10 \\sim C13 \\sim C11 \\sim C12 \\sim C15 \\sim C16 \\sim F2 \\sim C11A \\sim
C12A \\sim C15A \\sim C16A \\sim F2A: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim F1 \\sim C3A \\sim C4A
\\sim C5A \\sim C6A \\sim C7A \\sim F1A \\sim C8: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C19 \\sim N1 \\sim C17 \\sim C18 \\sim C20 \\sim C21 \\sim C17A \\sim C18A
\\sim C20A \\sim C21A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(S1) = Uanis(N2)
5. Same fragment restrains
{C2, C8, C3A, C4A, C5A, C6A, C7A, F1A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C2, C8, C3, C4, C5, C6, C7, F1}
{C10, C13, C11A, C12A, C15A, C16A, F2A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C10, C13, C11, C12, C15, C16, F2}
{C19, N1, C17A, C18A, C20A, C21A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C19, N1, C17, C18, C20, C21}
6. Others
 Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=
 Sof(F1A)=1-FVAR(1)
 Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(F1)=FVAR(1)
 Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=
 Sof(F2A)=1-FVAR(2)
 Sof(C11)=Sof(H11)=Sof(C12)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(F2)=FVAR(2)
 Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=
 Sof(H21A)=1-FVAR(3)
 Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=FVAR(3)
 Sof(N2)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=0.5*(1-FVAR(5))
 Sof(S1)=0.5*FVAR(5)
7.a Riding coordinates:
 C22(H22A,H22B,H22C)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C11(H11), C15(H15), C16(H16), C17(H17), C18(H18),
 C20(H20), C21(H21), C3A(H3A), C4A(H4A), C6A(H6A), C11A(H11A), C15A(H15A),
 C16A(H16A), C17A(H17A), C18A(H18A), C20A(H20A), C21A(H21A)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 348 electrons were 
found in a volume of 1212\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C3H7NO] per Asymmetric Unit 
which account for 320 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              90926
_shelx_hkl_checksum              2925
_shelx_fab_checksum              44764
_olex2_submission_special_instructions 'No special instructions were received'