Proton-conducting coordination polymers formed from bipyridine phosphonate ligands
Ramteke, Prajakta Mohan; Plecháček, Tomáš; Kloda, Matous; Rohlíček, Jan; Vykydalová, Anna; Melanova, Klara; Bavol, Dmytro; Škoch, Karel; Taddei, Marco; Demel, Jan; Hynek, Jan; Dalton Transactions  (2026) –; doi:10.1039/D5DT02997J

data_7720591
_publ_section_title
;
 Proton-conducting coordination polymers formed from bipyridine
 phosphonate ligands.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5622
_journal_page_last               5634
_journal_paper_doi               10.1039/d5dt02997j
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C18 H26 N2 O6 P2'
_chemical_formula_sum            'C18 H26 N2 O6 P2'
_chemical_formula_weight         428.35
_chemical_name_systematic
'tetraethyl 4,4?-bipyridine-3,3?-bisphosphonate'
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-11-18
_audit_creation_method
;
Olex2 1.5-ac7-014
(compiled 2025.02.27 svn.r6f4c0eaf for Rigaku Oxford Diffraction, GUI svn.r7171)
;
_audit_update_record
;
2025-11-18 deposited with the CCDC.	2026-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.935(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6820(2)
_cell_length_b                   25.8378(5)
_cell_length_c                   8.43670(10)
_cell_measurement_reflns_used    13404
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      78.2930
_cell_measurement_theta_min      3.4560
_cell_volume                     2072.22(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.62a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.62a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.62a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac7-014 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-014 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_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    -80.00  14.00   0.50    0.50    --  -49.39 102.00-104.00  188
  2  \w    -80.00  14.00   0.50    0.50    --  -49.39 102.00-104.00  188
  3  \w      8.00  81.00   0.50    0.50    --   49.39-102.00 152.00  146
  4  \w    -81.00 -20.00   0.50    2.00    --  -90.00 102.00-104.00  122
  5  \w     42.00 107.00   0.50    2.00    --  111.50-102.00 152.00  130
  6  \w    106.00 178.00   0.50    2.00    --  111.50 102.00-104.00  144
  7  \w    -41.00  23.00   0.50    0.50    --  -49.39  37.00  60.00  128
  8  \w    -22.00  24.00   0.50    0.50    --  -49.39  19.00   0.00   92
  9  \w    -22.00  24.00   0.50    0.50    --  -49.39  19.00 -90.00   92
 10  \w    -23.00  22.00   0.50    0.50    --   49.39 -19.00-120.00   90
 11  \w    -23.00  22.00   0.50    0.50    --   49.39 -19.00-150.00   90
 12  \w    -50.00 -18.00   0.50    2.00    --  -90.00  45.00-180.00   64
 13  \w   -161.00-121.00   0.50    2.00    --  -90.00 -45.00 -90.00   80
 14  \w   -160.00-109.00   0.50    2.00    --  -90.00-102.00 152.00  102
 15  \w    113.00 159.00   0.50    2.00    --  111.50 125.00  30.00   92
 16  \w    125.00 168.00   0.50    2.00    --  111.50  45.00-180.00   86
 17  \w     41.00  72.00   0.50    2.00    --  111.50 -94.00-180.00   62
 18  \w     74.00 100.00   0.50    2.00    --  111.50 -94.00-180.00   52
 19  \w    126.00 178.00   0.50    2.00    --  111.50  61.00 150.00  104
 20  \w     44.00  79.00   0.50    2.00    --  111.50-125.00 -90.00   70
 21  \w     45.00 105.00   0.50    2.00    --  111.50 -94.00-150.00  120
 22  \w     47.00  72.00   0.50    2.00    --  111.50 -61.00-150.00   50
 23  \w     42.00  72.00   0.50    2.00    --  111.50 -61.00 -90.00   60
 24  \w    126.00 178.00   0.50    2.00    --  111.50  77.00   0.00  104
 25  \w     45.00  71.00   0.50    2.00    --  111.50 -61.00  60.00   52
 26  \w    127.00 159.00   0.50    2.00    --  111.50  61.00-120.00   64
 27  \w    125.00 170.00   0.50    2.00    --  111.50  77.00-150.00   90
 28  \w     42.00  70.00   0.50    2.00    --  111.50 -61.00 120.00   56
 29  \w    128.00 170.00   0.50    2.00    --  111.50  61.00 120.00   84
 30  \w     41.00  66.00   0.50    2.00    --  111.50 -61.00 150.00   50
 31  \w    125.00 177.00   0.50    2.00    --  111.50  77.00 -30.00  104
 32  \w     69.00  95.00   0.50    2.00    --  111.50 -94.00-120.00   52
 33  \w     41.00  66.00   0.50    2.00    --  111.50 -61.00 -30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0764385000
_diffrn_orient_matrix_UB_12      0.0521573000
_diffrn_orient_matrix_UB_13      0.0373568000
_diffrn_orient_matrix_UB_21      -0.0923325000
_diffrn_orient_matrix_UB_22      0.0238778000
_diffrn_orient_matrix_UB_23      -0.1511876000
_diffrn_orient_matrix_UB_31      -0.1090234000
_diffrn_orient_matrix_UB_32      0.0162622000
_diffrn_orient_matrix_UB_33      0.1017442000
_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  0.0562
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            21244
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.009
_diffrn_reflns_theta_min         3.421
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.232
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.62a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       irregular
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.437
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.106
_refine_diff_density_max         1.010
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0967P)^2^+1.2349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1526
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4071
_reflns_number_total             4407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02997j2.cif
_cod_data_source_block           pp-cii_00
_cod_depositor_comments
'Adding full bibliography for 7720590--7720593.cif.'
_cod_database_code               7720591
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'P2 O6 C18 H26 N2'
_shelx_estimated_absorpt_t_max   0.798
_shelx_estimated_absorpt_t_min   0.442
_diffrn_oxdiff_digest_hkl
;
01e85caa2034a9cdcf863912abd1e560e9d4f7
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H17A)=Sof(H17B)=Sof(C18B)=Sof(H18A)=Sof(H18B)=Sof(H18C)=1-FVAR(1)
 Sof(H17C)=Sof(H17D)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C11(H11A,H11B), C17(H17A,H17B), C17(H17C,H17D)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C10(H10), C9(H9), C1(H1), C2(H2)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C18B(H18A,H18B,
 H18C), C18A(H18D,H18E,H18F)
;
_shelx_res_checksum              23793
_shelx_hkl_checksum              98611
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.093
_oxdiff_exptl_absorpt_empirical_full_min 0.539