Zn(II) Three-Dimensional Metal-Organic Frameworks Based on 2,5-Diiodoterephthalate and N,N Linkers: Structures and Features of Sorption Behavior
Zaguzin, Alexander S.; Sukhikh, Taisiya; Sokolov, Maxim N.; Fedin, Vladimir P.; Adonin, Sergey A.; Inorganics 11 (2023) 192–; doi:10.3390/inorganics11050192

data_1569040
_publ_section_title
;
 Zn(II) Three-Dimensional Metal-Organic Frameworks Based on
 2,5-Diiodoterephthalate and N,N Linkers: Structures and Features of
 Sorption Behavior
;
_journal_issue                   5
_journal_name_full               Inorganics
_journal_page_first              192
_journal_paper_doi               10.3390/inorganics11050192
_journal_volume                  11
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         '0.13(C160 H112 I16 N16 O32 Zn8), C3 H7 N O'
_chemical_formula_sum            'C23 H21 I2 N3 O5 Zn'
_chemical_formula_weight         738.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   28.7667(10)
_cell_length_b                   31.0967(11)
_cell_length_c                   22.7773(8)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.53
_cell_measurement_theta_min      2.22
_cell_volume                     20375.4(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            53782
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.685
_diffrn_reflns_theta_min         1.315
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    3.427
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0746 before and 0.0681 after correction. The Ratio of minimum to maximum transmission is 0.8529. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_description       block
_exptl_crystal_F_000             11392
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.849
_refine_diff_density_min         -1.227
_refine_diff_density_rms         0.166
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         9670
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+522.6339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1565
_reflns_Friedel_coverage         0.948
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7378
_reflns_number_total             9670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZA-58_2_a.cif
_cod_data_source_block           za-58_2_a
_cod_database_code               1569040
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.795
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(5)
 0.50(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N5-C14 = C14-C13 = C13-C12 = C12-C11 = C11-C10 = N5-C10
 1.39 with sigma of 0.02
 C38-C37 = C9A-C15A = C9-C15 = C9A-C12A = C15-C12 = C9-C7 = C7A-C15A
 1.5 with sigma of 0.02
 C13A-C9A \\sim C9A-C11A
 with sigma of 0.02
4. Restrained planarity
 N4A, C4A, C5A, C6A, C7A, C8A, C9A
 with sigma of 0.1
 N4A, C4A, C5A, C6A, C7A, C8A, C15A
 with sigma of 0.1
 N5A, C10A, C11A, C12A, C13A, C14A
 with sigma of 0.1
 N5, C10, C11, C12, C13, C14
 with sigma of 0.1
 N4, C4, C5, C6, C7, C8, C9A
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C14) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(C6A) = Uiso(N5A) = Uiso(C10A) = Uiso(C14A) = Uiso(C11A) = Uiso(C13A) =
Uiso(C12A) = Uiso(C9A) = Uiso(C15A) = Uiso(C7A) = Uiso(C8A) = Uiso(C4A) =
Uiso(C5A) = Uiso(N4A)
Uiso(N1S) = Uiso(C1S) = Uiso(O1S) = Uiso(C3S) = Uiso(C2S) = Uiso(C4S) =
Uiso(O2S) = Uiso(N2S) = Uiso(C5S) = Uiso(C6S)
6. Rigid body (RIGU) restrains
 N3, O8, C1, C2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, C10, C11, C12, C13, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C4, C8, C7, C6, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(C4S)=Sof(H4S)=Sof(O2S)=Sof(N2S)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=Sof(H5SC)=
 Sof(C6S)=Sof(H6SA)=Sof(H6SB)=Sof(H6SC)=1-FVAR(1)
 Sof(C1S)=Sof(H1S)=Sof(O1S)=Sof(N1S)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(H2SC)=
 Sof(C3S)=Sof(H3SA)=Sof(H3SB)=Sof(H3SC)=FVAR(1)
 Sof(N4A)=Sof(C4A)=Sof(H4A)=Sof(C8A)=Sof(H8A)=Sof(C7A)=Sof(C6A)=Sof(H6A)=
 Sof(C5A)=Sof(H5A)=Sof(N5A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=
 Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C15A)=
 Sof(H15C)=Sof(H15D)=1-FVAR(2)
 Sof(N4)=Sof(C4)=Sof(H4)=Sof(C8)=Sof(H8)=Sof(C7)=Sof(C6)=Sof(H6)=Sof(C5)=
 Sof(H5)=Sof(N5)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=
 Sof(C12)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 FVAR(2)
8.a Free rotating group:
 C1S(O1S,N1S,C2S,C3S), C4S(O2S,N2S,C5S,C6S)
8.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C9(H9A,H9B), C9A(H9AA,H9AB), C15(H15A,H15B),
 C15A(H15C,H15D)
8.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C30(H30), C32(H32), C33(H33), C35(H35), C36(H36), C40(H40),
 C41(H41), C42(H42), C43(H43), C4(H4), C8(H8), C6(H6), C5(H5), C4A(H4A),
 C8A(H8A), C6A(H6A), C5A(H5A), C10A(H10A), C11A(H11A), C13A(H13A), C14A(H14A),
 C10(H10), C11(H11), C13(H13), C14(H14), C18(H18), C22(H22), C1S(H1S), C4S(H4S),
  C1(H1)
8.d Fitted hexagon refined as free rotating group:
 N4(C4,C8,C7,C6,C5), N4A(C4A,C8A,C7A,C6A,C5A), N5A(C10A,C11A,C12A,C13A,C14A)
8.e Idealised Me refined with riding coordinates:
 C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC), C5S(H5SA,H5SB,H5SC), C6S(H6SA,H6SB,
 H6SC)
8.f Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              24546
_shelx_hkl_checksum              31945
_olex2_submission_special_instructions 'No special instructions were received'