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_1569041
_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 H96 I16 N16 O32 Zn8), C3 H7 N O'
_chemical_formula_sum            'C23 H19 I2 N3 O5 Zn'
_chemical_formula_weight         736.58
_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             2022-11-03
_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                   28.6666(11)
_cell_length_b                   31.2803(15)
_cell_length_c                   22.6871(11)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.22
_cell_volume                     20343.5(16)
_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 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48728
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         1.927
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    3.432
_exptl_absorpt_correction_T_max  0.7434
_exptl_absorpt_correction_T_min  0.6911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0954 before and 0.0625 after correction. The Ratio of minimum to maximum transmission is 0.9296. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_description       block
_exptl_crystal_F_000             11328
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.669
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         9651
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0363P)^2^+338.5284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0999
_reflns_Friedel_coverage         0.948
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                8420
_reflns_number_total             9651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZA87new_a.cif
_cod_data_source_block           za87new_a
_cod_database_code               1569041
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.821
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.55(3)
 0.45(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N6-C45 = N6-C46
 1.45 with sigma of 0.02
 C45-C46
 2.3 with sigma of 0.04
 N7-C48 \\sim N7-C49
 with sigma of 0.02
 C46-C44 \\sim C44-C45
 with sigma of 0.02
4. Restrained planarity
 O11, N7, C47, C48, C49
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(C41) \\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uiso(C48) = Uiso(C47) = Uiso(O11) = Uiso(N7) = Uiso(C49)
6. Rigid body (RIGU) restrains
 N4, C32, C36, C38, C41, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(C47)=Sof(H47)=Sof(O11)=Sof(N7)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(H48C)=
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=1-FVAR(1)
 Sof(O10)=Sof(N6)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(1)
8.a Free rotating group:
 C47(O11,N7,C48,C49)
8.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C15(H15), C18(H18), C20(H20), C21(H21), C24(H24), C26(H26),
 C27(H27), C28(H28), C29(H29), C31(H31), C3(H3), C14(H14), C25(H25), C30(H30),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C43(H43),
  C17(H17), C44(H44), C47(H47)
8.c Idealised Me refined with riding coordinates:
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,
 H49C)
8.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              83056
_shelx_hkl_checksum              67650
_olex2_submission_special_instructions 'No special instructions were received'