Amidinium⋯phosphonate charge assisted hydrogen-bonded organic frameworks: influence of diverse intermolecular interactions
Almuhana, Asia R. Y.; Griffin, Sarah L.; Champness, Neil R.; CrystEngComm 26 (2024) 4643–4648; doi:10.1039/D4CE00479E

data_7249130
_publ_section_title
;
 Amidinium&#x22EF;phosphonate charge assisted hydrogen-bonded organic
 frameworks: influence of diverse intermolecular interactions
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              4643
_journal_page_last               4648
_journal_paper_doi               10.1039/D4CE00479E
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         '2(C28 H16 N2 O11 P2), 5(C8 H12 N4), 40[H2O]'
_chemical_formula_sum            'C96 H172 N24 O62 P4'
_chemical_formula_weight         2778.45
_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
_audit_creation_date             2024-04-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-03 deposited with the CCDC.	2024-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                92.9800(10)
_cell_angle_beta                 92.5630(10)
_cell_angle_gamma                102.7010(10)
_cell_formula_units_Z            1
_cell_length_a                   10.74890(10)
_cell_length_b                   11.10920(10)
_cell_length_c                   28.1083(2)
_cell_measurement_reflns_used    58769
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.8560
_cell_measurement_theta_min      3.1210
_cell_volume                     3264.47(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.960
_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   -119.00 -54.00   0.50    1.85    --  -47.48-153.00 162.00  130
  2  \w    -84.00 -10.00   0.50    1.85    --  -47.48 121.00  43.00  148
  3  \w   -105.00 -27.00   0.50    1.85    --  -47.48 153.00-157.00  156
  4  \w     32.00  92.00   0.50    1.85    --   47.48-121.00 -38.00  120
  5  \w     49.00 111.00   0.50    1.85    --   47.48-153.00 162.00  124
  6  \w    -84.00 -18.00   0.50    7.42    --  -90.00 121.00  43.00  132
  7  \w   -147.00 -54.00   0.50    7.42    --  -90.00-153.00 162.00  186
  8  \w   -161.00 -76.00   0.50    7.42    --  -90.00-121.00 -38.00  170
  9  \w     49.00 131.00   0.50    7.42    --  110.64-153.00 162.00  164
 10  \w     40.00 110.00   0.50    7.42    --  110.64-121.00 -38.00  140
 11  \w     76.00 164.00   0.50    7.42    --  110.64 153.00-157.00  176
 12  \w     98.00 178.00   0.50    7.42    --  110.64 121.00  43.00  160
 13  \w    -34.00  27.00   0.50    1.85    --  -47.48  19.00  90.00  122
 14  \w    -34.00  27.00   0.50    1.85    --  -47.48  19.00 -30.00  122
 15  \w   -120.00 -37.00   0.50    1.85    --  -47.48 -38.00-180.00  166
 16  \w    -34.00  27.00   0.50    1.85    --  -47.48  19.00   0.00  122
 17  \w    -26.00  26.00   0.50    1.85    --   47.48 -19.00 -90.00  104
 18  \w    -26.00  26.00   0.50    1.85    --   47.48 -19.00-150.00  104
 19  \w    -26.00  26.00   0.50    1.85    --   47.48 -19.00  60.00  104
 20  \w    -69.00 -18.00   0.50    7.42    --  -90.00  57.00 -90.00  102
 21  \w    -48.00 -18.00   0.50    7.42    --  -90.00  38.00  90.00   60
 22  \w    -48.00 -18.00   0.50    7.42    --  -90.00  38.00 -30.00   60
 23  \w    -69.00 -18.00   0.50    7.42    --  -90.00  57.00-150.00  102
 24  \w   -163.00 -79.00   0.50    7.42    --  -90.00 -19.00   0.00  168
 25  \w   -161.00-105.00   0.50    7.42    --  -90.00 -77.00-180.00  112
 26  \w    -48.00 -18.00   0.50    7.42    --  -90.00  38.00   0.00   60
 27  \w    -69.00 -18.00   0.50    7.42    --  -90.00  57.00-180.00  102
 28  \w    -48.00 -18.00   0.50    7.42    --  -90.00  38.00-180.00   60
 29  \w    -85.00 -18.00   0.50    7.42    --  -90.00 125.00  90.00  134
 30  \w    -69.00 -18.00   0.50    7.42    --  -90.00  57.00   0.00  102
 31  \w   -161.00 -94.00   0.50    7.42    --  -90.00 -57.00  30.00  134
 32  \w   -161.00-105.00   0.50    7.42    --  -90.00 -77.00 -90.00  112
 33  \w   -161.00 -94.00   0.50    7.42    --  -90.00 -57.00-120.00  134
 34  \w     40.00 106.00   0.50    7.42    --  110.64 -99.00  60.00  132
 35  \w     40.00 106.00   0.50    7.42    --  110.64 -99.00-150.00  132
 36  \w     40.00  97.00   0.50    7.42    --  110.64 -77.00   0.00  114
 37  \w     40.00 106.00   0.50    7.42    --  110.64 -99.00 -60.00  132
 38  \w     40.00 106.00   0.50    7.42    --  110.64 -99.00 120.00  132
 39  \w     40.00  97.00   0.50    7.42    --  110.64 -77.00 -30.00  114
 40  \w     40.00  97.00   0.50    7.42    --  110.64 -77.00 120.00  114
 41  \w     40.00 106.00   0.50    7.42    --  110.64 -99.00-180.00  132
 42  \w     40.00 106.00   0.50    7.42    --  110.64 -99.00-120.00  132
 43  \w     40.00 111.00   0.50    7.42    --  110.64-125.00  60.00  142
 44  \w    105.00 178.00   0.50    7.42    --  110.64  77.00  90.00  146
 45  \w     40.00 111.00   0.50    7.42    --  110.64-125.00 -90.00  142
 46  \w   -120.00 -37.00   0.50    1.85    --  -47.48 -38.00 -60.00  166
 47  \w   -120.00 -37.00   0.50    1.85    --  -47.48 -38.00 120.00  166
 48  \w   -120.00 -37.00   0.50    1.85    --  -47.48 -38.00 -90.00  166
 49  \w   -120.00 -37.00   0.50    1.85    --  -47.48 -38.00 -30.00  166
 50  \w   -120.00 -37.00   0.50    1.85    --  -47.48 -38.00  90.00  166
 51  \w   -120.00 -37.00   0.50    1.85    --  -47.48 -38.00-150.00  166
 52  \w   -120.00 -37.00   0.50    1.85    --  -47.48 -38.00  60.00  166
 53  \w   -120.00 -37.00   0.50    1.85    --  -47.48 -38.00   0.00  166
 54  \w   -120.00 -37.00   0.50    1.85    --  -47.48 -38.00-120.00  166
 55  \w   -120.00 -37.00   0.50    1.85    --  -47.48 -38.00  30.00  166
 56  \w   -162.00 -79.00   0.50    7.42    --  -90.00 -38.00 120.00  166
 57  \w   -162.00 -79.00   0.50    7.42    --  -90.00 -38.00  60.00  166
 58  \w   -162.00 -79.00   0.50    7.42    --  -90.00 -38.00 -30.00  166
 59  \w    -48.00 -18.00   0.50    7.42    --  -90.00  38.00 150.00   60
 60  \w    -48.00 -18.00   0.50    7.42    --  -90.00  38.00  30.00   60
 61  \w   -162.00 -79.00   0.50    7.42    --  -90.00 -38.00 -60.00  166
 62  \w   -162.00 -79.00   0.50    7.42    --  -90.00 -38.00-180.00  166
 63  \w   -162.00 -79.00   0.50    7.42    --  -90.00 -38.00  30.00  166
 64  \w   -162.00 -79.00   0.50    7.42    --  -90.00 -38.00-150.00  166
 65  \w   -162.00 -79.00   0.50    7.42    --  -90.00 -38.00  90.00  166
 66  \w   -162.00 -79.00   0.50    7.42    --  -90.00 -38.00   0.00  166
 67  \w    -48.00 -18.00   0.50    7.42    --  -90.00  38.00-120.00   60
 68  \w   -162.00 -79.00   0.50    7.42    --  -90.00 -38.00 -90.00  166
 69  \w   -162.00 -79.00   0.50    7.42    --  -90.00 -38.00 150.00  166
 70  \w   -162.00 -79.00   0.50    7.42    --  -90.00 -38.00-120.00  166
 71  \w     97.00 172.00   0.50    7.42    --  110.64  57.00  90.00  150
 72  \w     97.00 178.00   0.50    7.42    --  110.64  57.00 -60.00  162
 73  \w     97.00 178.00   0.50    7.42    --  110.64  57.00-150.00  162
 74  \w     97.00 178.00   0.50    7.42    --  110.64  57.00  60.00  162
 75  \w     97.00 178.00   0.50    7.42    --  110.64  57.00-180.00  162
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            117847
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.569
_diffrn_reflns_theta_min         3.154
_exptl_absorpt_coefficient_mu    1.448
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         13490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0923
_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/[\s^2^(Fo^2^)+(0.1175P)^2^+13.8525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2687
_refine_ls_wR_factor_ref         0.2732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12113
_reflns_number_total             13490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00479e2.cif
_cod_data_source_block           ara_hof_pndi_7_mask
_cod_depositor_comments
'Adding full bibliography for 7249127--7249130.cif.'
_cod_database_code               7249130
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.881
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2.a Rotating group:
 N2B(H2BA,H2BB)
2.b Secondary CH2 refined with riding coordinates:
 C1P(H1PA,H1PB), C28P(H28A,H28B)
2.c Aromatic/amide H refined with riding coordinates:
 C3P(H3P), C4P(H4P), C6P(H6P), C7P(H7P), C10P(H10P), C11P(H11P), C15P(H15P),
 C16P(H16P), C23P(H23P), C24P(H24P), C26P(H26P), C27P(H27P), C3A(H3A), C4A(H4A),
  C6A(H6A), C7A(H7A), C3B(H3B), C4B(H4B), C6B(H6B), C7B(H7B), C3C(H3C), C4C(H4C)
2.d X=CH2 refined with riding coordinates:
 N1A(H1AA,H1AB), N2A(H2AA,H2AB), N3A(H3AA,H3AB), N4A(H4AA,H4AB), N1B(H1BA,
 H1BB), N3B(H3BA,H3BB), N4B(H4BA,H4BB), N1C(H1CA,H1CB), N2C(H2CA,H2CB)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 407 electrons were 
found in a volume of 1184\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
40[H2O] per formula unit 
which account for 400 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              49584
_shelx_hkl_checksum              9088
_shelx_fab_checksum              75408
_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
;