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_7063800
_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         'C12 H10 Cl N2 O5 S, H4 N'
_chemical_formula_sum            'C12 H14 Cl N3 O5 S'
_chemical_formula_weight         347.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 91.2793(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.18826(7)
_cell_length_b                   4.75496(4)
_cell_length_c                   36.8598(3)
_cell_measurement_reflns_used    32131
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      74.7440
_cell_measurement_theta_min      4.7590
_cell_volume                     1434.77(2)
_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 0.996
_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    -91.00  -9.00   1.00    1.00    --  -41.63 130.00-129.00   82
  2  \w   -115.00 -68.00   1.00    1.00    --  -41.63-139.00 -16.00   47
  3  \w     30.00 100.00   1.00    1.00    --   41.63-130.00 158.00   70
  4  \w     37.00 116.00   1.00    4.00    --  108.63-130.00 158.00   79
  5  \w     35.00 123.00   1.00    4.00    --  108.63-139.00 -16.00   88
  6  \w     35.00 123.00   1.00    4.00    --  108.63-139.00 -16.00   88
  7  \w     94.00 178.00   1.00    4.00    --  108.63 130.00-129.00   84
  8  \w     90.00 174.00   1.00    4.00    --  108.63 139.00  44.00   84
  9  \w   -115.00 -13.00   1.00    1.00    --  -41.63 -57.00  60.00  102
 10  \w   -115.00 -13.00   1.00    1.00    --  -41.63 -57.00  30.00  102
 11  \w    -87.00  -6.00   1.00    1.00    --  -41.63 125.00 150.00   81
 12  \w   -115.00 -13.00   1.00    1.00    --  -41.63 -57.00 -90.00  102
 13  \w   -115.00 -13.00   1.00    1.00    --  -41.63 -57.00  60.00  102
 14  \w   -115.00 -13.00   1.00    1.00    --  -41.63 -57.00  30.00  102
 15  \w   -115.00 -13.00   1.00    1.00    --  -41.63 -57.00 -30.00  102
 16  \w   -115.00 -13.00   1.00    1.00    --  -41.63 -57.00 -30.00  102
 17  \w   -115.00 -13.00   1.00    1.00    --  -41.63 -57.00 -90.00  102
 18  \w    -70.00  32.00   1.00    1.00    --  -41.63  57.00  30.00  102
 19  \w   -116.00 -17.00   1.00    1.00    --  -41.63 -37.00-150.00   99
 20  \w   -115.00 -13.00   1.00    1.00    --  -41.63 -57.00 150.00  102
 21  \w     10.00  36.00   1.00    1.00    --   41.63  73.00  -8.74   26
 22  \w      8.00  42.00   1.00    1.00    --   41.63  82.00-127.86   34
 23  \w      7.00  33.00   1.00    1.00    --   41.63  84.00  71.63   26
 24  \w     35.00 106.00   1.00    1.00    --   41.63-139.00 -16.00   71
 25  \w     80.00 178.00   1.00    4.00    --  108.63  61.00-120.00   98
 26  \w     80.00 178.00   1.00    4.00    --  108.63  61.00  30.00   98
 27  \w     83.00 178.00   1.00    4.00    --  108.63  45.00 -60.00   95
 28  \w     26.00 106.00   1.00    4.00    --  108.63 -94.00 -30.00   80
 29  \w     80.00 178.00   1.00    4.00    --  108.63  61.00 -60.00   98
 30  \w     80.00 178.00   1.00    4.00    --  108.63  61.00 -90.00   98
 31  \w     83.00 178.00   1.00    4.00    --  108.63  45.00 -60.00   95
 32  \w     80.00 178.00   1.00    4.00    --  108.63  61.00 -90.00   98
 33  \w     83.00 178.00   1.00    4.00    --  108.63  45.00  90.00   95
 34  \w     80.00 178.00   1.00    4.00    --  108.63  61.00 -30.00   98
 35  \w     37.00 113.00   1.00    4.00    --  108.63-125.00-120.00   76
 36  \w     83.00 178.00   1.00    4.00    --  108.63  45.00 120.00   95
 37  \w     37.00 113.00   1.00    4.00    --  108.63-125.00  60.00   76
 38  \w     83.00 178.00   1.00    4.00    --  108.63  45.00   0.00   95
 39  \w     80.00 178.00   1.00    4.00    --  108.63  61.00  90.00   98
 40  \w     80.00 178.00   1.00    4.00    --  108.63  61.00   0.00   98
 41  \w     80.00 178.00   1.00    4.00    --  108.63  61.00-150.00   98
 42  \w     80.00 178.00   1.00    4.00    --  108.63  61.00-180.00   98
 43  \w     80.00 178.00   1.00    4.00    --  108.63  61.00 120.00   98
 44  \w     36.00 138.00   1.00    4.00    --  108.63 -61.00 120.00  102
 45  \w     80.00 178.00   1.00    4.00    --  108.63  61.00  60.00   98
 46  \w     37.00 113.00   1.00    4.00    --  108.63-125.00  90.00   76
 47  \w     83.00 178.00   1.00    4.00    --  108.63  45.00-180.00   95
 48  \w     80.00 178.00   1.00    4.00    --  108.63  61.00-120.00   98
 49  \w     80.00 178.00   1.00    4.00    --  108.63  61.00 150.00   98
 50  \w   -116.00 -17.00   1.00    1.00    --  -41.63 -37.00 -90.00   99
 51  \w   -116.00 -17.00   1.00    1.00    --  -41.63 -37.00-120.00   99
 52  \w   -115.00 -13.00   1.00    1.00    --  -41.63 -57.00  90.00  102
 53  \w   -116.00 -17.00   1.00    1.00    --  -41.63 -37.00 150.00   99
 54  \w    -47.00 130.00   1.00    1.00    --   41.63   0.00   0.00  177
 55  \w    -47.00 130.00   1.00    1.00    --   41.63   0.00-180.00  177
 56  \w    -47.00 130.00   1.00    1.00    --   41.63   0.00 -30.00  177
 57  \w    -47.00 130.00   1.00    1.00    --   41.63   0.00 -90.00  177
 58  \w    -47.00 130.00   1.00    1.00    --   41.63   0.00-120.00  177
 59  \w    -47.00 130.00   1.00    1.00    --   41.63   0.00 -60.00  177
 60  \w    -47.00 130.00   1.00    1.00    --   41.63   0.00-150.00  177
 61  \w     10.00  36.00   1.00    1.00    --   41.63  72.00 -63.28   26
 62  \w      8.00  42.00   1.00    1.00    --   41.63  80.00 168.24   34
;
_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      0.0359258000
_diffrn_orient_matrix_UB_12      -0.0592884000
_diffrn_orient_matrix_UB_13      0.0404913000
_diffrn_orient_matrix_UB_21      -0.1055766000
_diffrn_orient_matrix_UB_22      0.2545602000
_diffrn_orient_matrix_UB_23      0.0103575000
_diffrn_orient_matrix_UB_31      -0.1515244000
_diffrn_orient_matrix_UB_32      -0.1914934000
_diffrn_orient_matrix_UB_33      0.0012331000
_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  0.1338
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            46249
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.731
_diffrn_reflns_theta_min         4.800
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.997
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39070
_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            colourless
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       needle
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2916
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0515P)^2^+2.2602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2863
_reflns_number_total             2916
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01438g2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7063799--7063801.cif.'
_cod_original_cell_volume        1434.78(2)
_cod_database_code               7063800
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.691
_shelx_estimated_absorpt_t_min   0.240
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(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)
;
_shelx_res_checksum              74814
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.716
_oxdiff_exptl_absorpt_empirical_full_min 0.435