The use of a dynamic solvent system as a novel approach to sustainable MOF crystallization
Shupletsov, Leonid; Schieck, Alina C.; Senkovska, Irena; Bon, Volodymyr; Kaskel, Stefan; Green Chemistry 27 (2025) 10218–10233; doi:10.1039/D5GC01029B

data_7250693
_publ_section_title
;
 The use of a dynamic solvent system as a novel approach to sustainable
 MOF crystallization
;
_journal_issue                   34
_journal_name_full               'Green Chemistry'
_journal_page_first              10218
_journal_page_last               10233
_journal_paper_doi               10.1039/D5GC01029B
_journal_volume                  27
_journal_year                    2025
_chemical_formula_sum            'C12 H8 N4 O0.5 Zn'
_chemical_formula_weight         281.59
_chemical_name_systematic        BUT-58
_space_group_crystal_system      tetragonal
_space_group_IT_number           98
_space_group_name_Hall           'I 4bw 2bw'
_space_group_name_H-M_alt        'I 41 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-02-23 deposited with the CCDC.	2025-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.3434(2)
_cell_length_b                   16.3434(2)
_cell_length_c                   12.5154(2)
_cell_measurement_reflns_used    17415
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      29.6060
_cell_measurement_theta_min      2.4970
_cell_volume                     3342.95(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.95a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.95a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.95a (Rigaku OD, 2023)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_detector_type            'Eiger2 1M'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Eiger2 1M'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22684
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.736
_diffrn_reflns_theta_min         2.492
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.459
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.95a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details
;
 Flack x determined using 826 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         2204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0916P)^2^+0.0326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.697
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.889
_reflns_number_gt                2083
_reflns_number_total             2204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5gc01029b3.cif
_cod_data_source_block           ACS4_16-BUT-1_auto
_cod_depositor_comments
'Adding full bibliography for 7250692--7250694.cif.'
_cod_original_cell_volume        3342.95(10)
_cod_original_formula_sum        'C12 H8 N4 O0.50 Zn'
_cod_database_code               7250693
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.844
_shelx_estimated_absorpt_t_max   0.892
_oxdiff_exptl_absorpt_empirical_full_min 0.871
_oxdiff_exptl_absorpt_empirical_full_max 1.242
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              84408
_shelx_hkl_checksum              15243