#------------------------------------------------------------------------------
#$Date: 2026-03-07 02:11:38 +0100 (Sat 07 de Mar de 2026) $
#$Revision: 304989 $
#$URL: svn://www.crystallography.net/cod/cif/7/72/05/7720590.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7720590
loop_
_publ_author_name
'Ramteke, Prajakta Mohan'
'Plecháček, Tomáš'
'Kloda, Matous'
'Rohlíček, Jan'
'Vykydalová, Anna'
'Melanova, Klara'
'Bavol, Dmytro'
'Škoch, Karel'
'Taddei, Marco'
'Demel, Jan'
'Hynek, Jan'
_publ_section_title
;
 Proton-conducting coordination polymers formed from bipyridine
 phosphonate ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D5DT02997J
_journal_year                    2026
_chemical_formula_moiety         'C5 H5 Mg N O4 P'
_chemical_formula_sum            'C5 H5 Mg N O4 P'
_chemical_formula_weight         198.38
_chemical_name_systematic
catena-(μ-4,4?-bipyridine-3,3?-diphosphonato)-aqua-magnesium(ii)
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2025-10-20
_audit_creation_method
;
Olex2 1.5-ac7-014
(compiled 2025.02.27 svn.r6f4c0eaf for Rigaku Oxford Diffraction, GUI svn.r7171)
;
_audit_update_record
;
2025-10-31 deposited with the CCDC.	2026-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.325(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3136(6)
_cell_length_b                   6.5320(4)
_cell_length_c                   13.3665(9)
_cell_measurement_reflns_used    1259
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.8190
_cell_measurement_theta_min      3.4840
_cell_volume                     684.96(9)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  16.00   0.50   20.30    --  -49.55  19.00 -30.00   50
  2  ω   -115.00 -80.00   0.50   20.30    --  -49.55-125.00 -30.00   70
  3  ω    -28.00  22.00   0.50   20.30    --  -49.55  38.00-120.00  100
  4  ω     52.00 108.00   0.50   20.30    --   49.55  38.00  90.00  112
  5  ω     88.00 116.00   0.50   20.30    --   49.55  77.00  90.00   56
  6  ω    -61.00 -30.00   0.50   81.19    --  -90.00  57.00 -30.00   62
  7  ω    -59.00 -25.00   0.50   81.19    --  -90.00  57.00 -90.00   68
  8  ω    -64.00 -21.00   0.50   81.19    --  -90.00  57.00 -60.00   86
  9  ω   -160.00 -83.00   0.50   81.19    --  -90.00 -19.00  60.00  154
 10  ω   -129.00-103.00   0.50   81.19    --  -90.00 -99.00  60.00   52
 11  ω    -66.00 -41.00   0.50   81.19    --  -90.00  57.00-180.00   50
 12  ω    -63.00 -29.00   0.50   81.19    --  -90.00  57.00-120.00   68
 13  ω    -86.00 -44.00   0.50   81.19    --  -90.00 125.00-120.00   84
 14  ω     41.00  66.00   0.50   81.19    --  107.39 -57.00  60.00   50
 15  ω    111.00 178.00   0.50   81.19    --  107.39  19.00 150.00  134
 16  ω    141.00 176.00   0.50   81.19    --  107.39 125.00 -30.00   70
 17  ω     92.00 127.00   0.50   81.19    --  107.39 125.00 -30.00   70
 18  ω     38.00  65.00   0.50   81.19    --  107.39 -57.00  90.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1866452000
_diffrn_orient_matrix_UB_12      -0.0294843000
_diffrn_orient_matrix_UB_13      0.0056002000
_diffrn_orient_matrix_UB_21      0.0609563000
_diffrn_orient_matrix_UB_22      0.1039379000
_diffrn_orient_matrix_UB_23      0.1095891000
_diffrn_orient_matrix_UB_31      0.0042249000
_diffrn_orient_matrix_UB_32      -0.2096966000
_diffrn_orient_matrix_UB_33      0.0536126000
_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  0.0212
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            1761
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.160
_diffrn_reflns_theta_min         3.504
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.282
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.833
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_description       plate
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.065
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.017
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         681
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0665P)²+0.7636P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                604
_reflns_number_total             681
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt02997j2.cif
_cod_data_source_block           ppciimg5_nontwin
_cod_database_code               7720590
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Mg P O4 C5 H5 N'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_diffrn_oxdiff_digest_hkl
;
019ad5b17f44a204779fc003851ffe08adc266
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H3A(0.5) H3B(0.5)
3.a Rotating group:
 O3(H3A,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C2(H2), C5(H5)
;
_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 3.751
_oxdiff_exptl_absorpt_empirical_full_min 0.787
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.78155(9) 0.000000 0.12708(6) 0.0140(3) Uani 1 2 d S T P . .
Mg1 Mg 1.15736(12) 0.000000 0.10598(7) 0.0145(3) Uani 1 2 d S T P . .
O3 O 1.4197(3) 0.000000 0.1704(2) 0.0245(6) Uani 1 2 d S T P . .
H3A H 1.462457 0.084240 0.135253 0.037 Uiso 0.5 1 d R U P . .
H3B H 1.459257 -0.119530 0.161093 0.037 Uiso 0.5 1 d R U P . .
C4 C 1.1927(4) 0.000000 0.4533(3) 0.0209(7) Uani 1 2 d S T P . .
H4 H 1.282927 0.000000 0.519250 0.025 Uiso 1 2 calc R U P . .
C2 C 0.8981(4) 0.000000 0.3504(2) 0.0188(7) Uani 1 2 d S T P . .
H2 H 0.780916 0.000000 0.344206 0.023 Uiso 1 2 calc R U P . .
C3 C 1.0225(4) 0.000000 0.4506(2) 0.0188(7) Uani 1 2 d S T P . .
C5 C 1.2285(4) 0.000000 0.3592(3) 0.0201(7) Uani 1 2 d S T P . .
H5 H 1.344683 0.000000 0.363119 0.024 Uiso 1 2 calc R U P . .
N1 N 1.1089(3) 0.000000 0.2629(2) 0.0166(6) Uani 1 2 d S T P . .
C1 C 0.9450(4) 0.000000 0.2590(2) 0.0165(7) Uani 1 2 d S T P . .
O1 O 0.8881(2) 0.000000 0.05393(16) 0.0167(5) Uani 1 2 d S T P . .
O2 O 0.67586(18) 0.1908(2) 0.12067(11) 0.0179(4) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 -1 0.0321
1 -1 0 0.0351
0 0 -1 0.0019
0 0 1 0.0155
-3 -3 -3 0.0205
5 0 0 0.0349
0 3 6 0.0326
0 -3 -6 0.0192
-3 -3 4 0.0214
0 -4 4 0.0278
3 3 -4 0.0240
-1 4 -4 0.0210
-5 0 3 0.0240
-4 2 0 0.0189
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 P1 C1 102.35(13) . . ?
O2 P1 C1 106.63(8) 6 . ?
O2 P1 C1 106.63(8) . . ?
O2 P1 O1 114.52(7) 6 . ?
O2 P1 O1 114.52(7) . . ?
O2 P1 O2 111.14(12) . 6 ?
O3 Mg1 Mg1 145.31(9) . 5_755 ?
O3 Mg1 N1 95.80(10) . . ?
O3 Mg1 O1 174.92(10) . . ?
N1 Mg1 Mg1 118.88(8) . 5_755 ?
O1 Mg1 Mg1 39.77(6) . 5_755 ?
O1 Mg1 Mg1 41.40(6) 5_755 5_755 ?
O1 Mg1 O3 103.92(10) 5_755 . ?
O1 Mg1 N1 160.28(10) 5_755 . ?
O1 Mg1 N1 79.12(9) . . ?
O1 Mg1 O1 81.16(9) 5_755 . ?
O2 Mg1 Mg1 95.77(5) 8 5_755 ?
O2 Mg1 Mg1 95.77(5) 3_545 5_755 ?
O2 Mg1 O3 85.63(5) 8 . ?
O2 Mg1 O3 85.63(5) 3_545 . ?
O2 Mg1 N1 86.64(5) 8 . ?
O2 Mg1 N1 86.64(5) 3_545 . ?
O2 Mg1 O1 94.76(5) 8 5_755 ?
O2 Mg1 O1 94.01(5) 3_545 . ?
O2 Mg1 O1 94.76(5) 3_545 5_755 ?
O2 Mg1 O1 94.01(5) 8 . ?
O2 Mg1 O2 168.38(10) 8 3_545 ?
C5 C4 C3 119.7(3) . . ?
C3 C2 C1 120.4(3) . . ?
C4 C3 C3 121.7(4) . 5_756 ?
C2 C3 C4 116.4(3) . . ?
C2 C3 C3 121.9(4) . 5_756 ?
N1 C5 C4 123.9(3) . . ?
C5 N1 Mg1 125.9(2) . . ?
C5 N1 C1 117.2(3) . . ?
C1 N1 Mg1 116.9(2) . . ?
C2 C1 P1 120.5(2) . . ?
N1 C1 P1 117.1(2) . . ?
N1 C1 C2 122.4(3) . . ?
P1 O1 Mg1 136.61(12) . 5_755 ?
P1 O1 Mg1 124.56(12) . . ?
Mg1 O1 Mg1 98.84(9) 5_755 . ?
P1 O2 Mg1 148.22(10) . 3_455 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1 1.836(3) . ?
P1 O1 1.521(2) . ?
P1 O2 1.5107(15) . ?
P1 O2 1.5108(15) 6 ?
Mg1 Mg1 3.1570(19) 5_755 ?
Mg1 O3 2.063(2) . ?
Mg1 N1 2.263(3) . ?
Mg1 O1 2.113(2) . ?
Mg1 O1 2.044(2) 5_755 ?
Mg1 O2 2.0303(15) 8 ?
Mg1 O2 2.0303(15) 3_545 ?
C4 C3 1.404(5) . ?
C4 C5 1.384(4) . ?
C2 C3 1.395(5) . ?
C2 C1 1.401(4) . ?
C3 C3 1.486(6) 5_756 ?
C5 N1 1.341(4) . ?
N1 C1 1.346(4) . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.9993 -0.0006 -0.9998 0.1809 -0.0487 -0.0493
1.0001 -1.0011 0.0008 0.2162 -0.0430 0.2142
-0.0003 0.0001 -1.0004 -0.0057 -0.1096 -0.0537
0.0003 -0.0001 1.0004 0.0057 0.1096 0.0537
-2.9979 -2.9989 -3.0024 -0.4879 -0.8235 0.4552
4.9978 -0.0035 0.0030 0.9329 0.3046 0.0220
0.0000 3.0007 6.0018 -0.0549 0.9696 -0.3075
-0.0000 -3.0007 -6.0018 0.0549 -0.9696 0.3075
-2.9961 -2.9995 4.0004 -0.4484 -0.0560 0.8308
0.0031 -4.0020 4.0024 0.1410 0.0228 1.0538
2.9961 2.9995 -4.0004 0.4484 0.0560 -0.8308
-1.0027 4.0027 -4.0030 -0.3276 -0.0838 -1.0582
-4.9970 0.0032 2.9982 -0.9160 0.0243 0.1390
-3.9993 2.0036 -0.0028 -0.8055 -0.0358 -0.4372
