Dipyridinophane ligands – synthesis and coordination study
Kuncová, Lucie; Lazarová, Jana; Kotek, Jan; Kubíček, Vojtěch; Hermann, Petr; RSC Advances 16 (2026) 18220–18231; doi:10.1039/D6RA00469E

data_7251863
_publ_section_title
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 Dipyridinophane ligands -- synthesis and coordination study
;
_journal_issue                   20
_journal_name_full               'RSC Advances'
_journal_page_first              18220
_journal_page_last               18231
_journal_paper_doi               10.1039/D6RA00469E
_journal_volume                  16
_journal_year                    2026
_chemical_formula_moiety         'C18 H18 Cl Fe N4 O4, 2(H2 O) [+ 2(H2 O)]'
_chemical_formula_sum            'C18 H26 Cl Fe N4 O8'
_chemical_formula_weight         517.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2026-02-20 deposited with the CCDC.	2026-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                72.604(5)
_cell_angle_beta                 72.489(5)
_cell_angle_gamma                63.055(5)
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_cell_length_a                   9.0585(12)
_cell_length_b                   9.7640(13)
_cell_length_c                   14.477(2)
_cell_measurement_reflns_used    9053
_cell_measurement_temperature    100(2)
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_cell_volume                     1068.4(3)
_computing_cell_refinement       'SAINT V8.41 (Bruker AXS LLC)'
_computing_data_collection       'Bruker Instrument Service v8.5.5.6'
_computing_data_reduction        'SAINT V8.41 (Bruker AXS LLC)'
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_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.391
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_max       12
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_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            86306
_diffrn_reflns_point_group_measured_fraction_full 1.000
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.322
_diffrn_reflns_theta_min         2.384
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\mS'
_exptl_absorpt_coefficient_mu    0.885
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for single-crystal
 structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       prism
_exptl_crystal_F_000             538
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.106
_platon_squeeze_void_content     '3Cl, 6(H2 O)'
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0242P)^2^+1.5796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5156
_reflns_number_total             5303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6ra00469e2.cif
_cod_data_source_block           py2n2_karboxfe2_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               7251863
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.794
_shelx_estimated_absorpt_t_max   0.912
_shelx_res_checksum              59331
_shelx_fab_checksum              62905