On zinc(ii) coordination chemistry with furosemide: a journey from a mononuclear complex to a coordination polymer
Podjed, Nina; Uranjek, Zarja; Cerc Korošec, Romana; Hrast Rambaher, Martina; Golob, Majda; Modec, Barbara; New Journal of Chemistry 49 (2025) 9113–9122; doi:10.1039/D5NJ01438G

data_7063801
_publ_section_title
;
 On zinc(ii) coordination chemistry with furosemide: a journey from a
 mononuclear complex to a coordination polymer
;
_journal_issue                   22
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9113
_journal_page_last               9122
_journal_paper_doi               10.1039/D5NJ01438G
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C64 H44 Cl2 N8 O18 S2 Zn3, 2(C H4 O)'
_chemical_formula_sum            'C66 H52 Cl2 N8 O20 S2 Zn3'
_chemical_formula_weight         1608.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-01-30 deposited with the CCDC.	2025-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.7000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0265(2)
_cell_length_b                   9.30170(10)
_cell_length_c                   34.3660(3)
_cell_measurement_reflns_used    18204
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      74.8570
_cell_measurement_theta_min      4.1920
_cell_volume                     6707.37(11)
_computing_cell_refinement       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4933
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -67.00  33.00   1.00    1.00    --  -41.76  32.00-171.00  100
  2  \w   -117.00 -44.00   1.00    1.00    --  -41.76 -32.00  29.00   73
  3  \w     69.00 114.00   1.00    1.00    --   41.76  32.00-171.00   45
  4  \w     36.00  64.00   1.00    2.00    --  108.63 -32.00  29.00   28
  5  \w     73.00 111.00   1.00    2.00    --  108.63 -32.00  29.00   38
  6  \w     90.00 176.00   1.00    2.00    --  108.63  32.00-171.00   86
  7  \w    -43.00  -8.00   1.00    1.00    --  -41.76 125.00 -90.00   35
  8  \w    -86.00  -8.00   1.00    1.00    --  -41.76 125.00-150.00   78
  9  \w     47.00  72.00   1.00    1.00    --   41.76-125.00-180.00   25
 10  \w     33.00  85.00   1.00    1.00    --   41.76-125.00  60.00   52
 11  \w     -7.00  18.00   1.00    1.00    --   41.76 -32.00  29.00   25
 12  \w     51.00  77.00   1.00    2.00    --  108.63-125.00-120.00   26
 13  \w    119.00 148.00   1.00    2.00    --  108.63  77.00  30.00   29
 14  \w     57.00 106.00   1.00    2.00    --  108.63 -94.00  60.00   49
 15  \w    121.00 178.00   1.00    2.00    --  108.63  77.00  60.00   57
 16  \w    114.00 140.00   1.00    2.00    --  108.63 125.00 120.00   26
 17  \w    143.00 178.00   1.00    2.00    --  108.63 125.00-120.00   35
 18  \w     48.00 113.00   1.00    2.00    --  108.63-125.00   0.00   65
 19  \w     37.00 131.00   1.00    2.00    --  108.63 -45.00 -60.00   94
 20  \w     87.00 112.00   1.00    2.00    --  108.63-125.00  60.00   25
 21  \w     87.00 112.00   1.00    2.00    --  108.63-125.00 -90.00   25
 22  \w     37.00  63.00   1.00    2.00    --  108.63-125.00 -90.00   26
 23  \w     87.00 113.00   1.00    2.00    --  108.63-125.00-120.00   26
 24  \w     84.00 177.00   1.00    2.00    --  108.63  45.00 120.00   93
 25  \w     45.00 118.00   1.00    2.00    --  108.63 -61.00 120.00   73
 26  \w     81.00 106.00   1.00    2.00    --  108.63 -94.00 -30.00   25
 27  \w     28.00  81.00   1.00    2.00    --  108.63 -94.00 -90.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0086990000
_diffrn_orient_matrix_UB_12      -0.1632022000
_diffrn_orient_matrix_UB_13      -0.0059154000
_diffrn_orient_matrix_UB_21      -0.0656572000
_diffrn_orient_matrix_UB_22      0.0084500000
_diffrn_orient_matrix_UB_23      0.0173351000
_diffrn_orient_matrix_UB_31      -0.0316819000
_diffrn_orient_matrix_UB_32      0.0271531000
_diffrn_orient_matrix_UB_33      -0.0410068000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            25467
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.787
_diffrn_reflns_theta_min         2.577
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.263
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.95a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       block
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         6803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+6.4242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6471
_reflns_number_total             6803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01438g2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7063799--7063801.cif.'
_cod_database_code               7063801
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.441
_shelx_estimated_absorpt_t_min   0.355
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C10A(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C12A(H12A), C13A(H13A), C14A(H14A), C15(H15), C21(H21), C22(H22),
 C23(H23), C24(H24), C26(H26), C27(H27), C31(H31), C32(H32), C33(H33), C34(H34),
  C36(H36), C37(H37)
2.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C)
;
_shelx_res_checksum              92435
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.651
_oxdiff_exptl_absorpt_empirical_full_min 0.637