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_7249129
_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         'C7 H7 O3 P, C4 H6 N2, 1[H2O]'
_chemical_formula_sum            'C11 H15 N2 O4 P'
_chemical_formula_weight         270.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-03-25
_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                90
_cell_angle_beta                 92.9890(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.0665(2)
_cell_length_b                   13.6291(3)
_cell_length_c                   15.2147(2)
_cell_measurement_reflns_used    11250
_cell_measurement_temperature    100.02(16)
_cell_measurement_theta_max      76.5760
_cell_measurement_theta_min      4.8610
_cell_volume                     2498.74(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_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    -75.00   0.00   0.50   10.00    --  -45.18 100.00 -58.00  150
  2  \w     -5.00  76.00   0.50   10.00    --   45.18-100.00-164.00  162
  3  \w    -92.00 -25.00   0.50   50.00    --  -97.00 100.00 -58.00  134
  4  \w     38.00  92.00   0.50   50.00    --  109.75-100.00-164.00  108
  5  \w    100.00 175.00   0.50   50.00    --  109.75 100.00 -58.00  150
  6  \w    -62.00 -34.00   0.50   10.00    --  -45.18 -56.00  51.84   56
  7  \w    -62.00 -34.00   0.50   10.00    --  -45.18 -55.00  78.16   56
  8  \w    -88.00 -16.00   0.50   10.00    --  -45.18 125.00   0.00  144
  9  \w    -62.00 -34.00   0.50   10.00    --  -45.18 -55.00 155.99   56
 10  \w    -30.00  15.00   0.50   10.00    --   45.18 -38.00-180.00   90
 11  \w    -27.00  41.00   0.50   10.00    --   45.18 -57.00 -60.00  136
 12  \w    -30.00  15.00   0.50   10.00    --   45.18 -38.00-150.00   90
 13  \w    -30.00  15.00   0.50   10.00    --   45.18 -38.00 -30.00   90
 14  \w    -27.00  41.00   0.50   10.00    --   45.18 -57.00-120.00  136
 15  \w    -30.00  15.00   0.50   10.00    --   45.18 -38.00  90.00   90
 16  \w    -93.00 -25.00   0.50   50.00    --  -97.00  97.00 -47.50  136
 17  \w    -97.00 -27.00   0.50   50.00    --  -97.00 114.00 101.82  140
 18  \w    -98.00 -27.00   0.50   50.00    --  -97.00 116.00 144.23  142
 19  \w    -92.00 -25.00   0.50   50.00    --  -97.00 100.00  92.09  134
 20  \w   -170.00 -86.00   0.50   50.00    --  -97.00 -54.00 -82.97  168
 21  \w    -55.00 -23.00   0.50   50.00    --  -97.00  61.00 -30.00   64
 22  \w    -97.00 -27.00   0.50   50.00    --  -97.00 115.00 -15.02  140
 23  \w    -92.00 -23.00   0.50   50.00    --  -97.00  94.00-122.23  138
 24  \w    -55.00 -23.00   0.50   50.00    --  -97.00  61.00   0.00   64
 25  \w   -140.00 -90.00   0.50   50.00    --  -97.00 -15.00 -90.00  100
 26  \w    -93.00 -25.00   0.50   50.00    --  -97.00  97.00 125.30  136
 27  \w    -92.00 -23.00   0.50   50.00    --  -97.00  95.00-154.34  138
 28  \w    -93.00 -25.00   0.50   50.00    --  -97.00  97.00  79.69  136
 29  \w   -168.00-106.00   0.50   50.00    --  -97.00-100.00-164.00  124
 30  \w    -97.00 -27.00   0.50   50.00    --  -97.00 114.00   4.13  140
 31  \w    -92.00 -25.00   0.50   50.00    --  -97.00  98.00 -93.34  134
 32  \w   -140.00 -90.00   0.50   50.00    --  -97.00 -15.00   0.00  100
 33  \w    -93.00 -25.00   0.50   50.00    --  -97.00 104.00-107.03  136
 34  \w    106.00 161.00   0.50   50.00    --  109.75  30.00 -90.00  110
 35  \w    104.00 131.00   0.50   50.00    --  109.75  15.00 150.00   54
 36  \w     38.00  93.00   0.50   50.00    --  109.75 -95.00  60.00  110
 37  \w    105.00 131.00   0.50   50.00    --  109.75  15.00-150.00   52
 38  \w     37.00  93.00   0.50   50.00    --  109.75 -95.00-120.00  112
 39  \w    104.00 132.00   0.50   50.00    --  109.75  15.00  90.00   56
 40  \w    105.00 132.00   0.50   50.00    --  109.75  15.00 -90.00   54
 41  \w     67.00  93.00   0.50   50.00    --  109.75 -95.00  30.00   52
 42  \w     99.00 174.00   0.50   50.00    --  109.75  77.00 150.00  150
 43  \w    107.00 132.00   0.50   50.00    --  109.75  15.00-180.00   50
 44  \w     55.00  93.00   0.50   50.00    --  109.75 -95.00   0.00   76
 45  \w     37.00  89.00   0.50   50.00    --  109.75 -95.00 120.00  104
 46  \w    142.00 168.00   0.50   50.00    --  109.75  77.00   0.00   52
 47  \w    105.00 132.00   0.50   50.00    --  109.75  15.00-120.00   54
 48  \w     99.00 124.00   0.50   50.00    --  109.75  77.00   0.00   50
 49  \w     37.00  71.00   0.50   50.00    --  109.75 -77.00  60.00   68
 50  \w     38.00  83.00   0.50   50.00    --  109.75 -95.00-150.00   90
 51  \w    111.00 160.00   0.50   50.00    --  109.75  30.00 -60.00   98
 52  \w    105.00 132.00   0.50   50.00    --  109.75  15.00 120.00   54
 53  \w     37.00  93.00   0.50   50.00    --  109.75 -95.00 150.00  112
 54  \w    106.00 131.00   0.50   50.00    --  109.75  15.00   0.00   50
 55  \w     43.00  87.00   0.50   50.00    --  109.75 -95.00 -90.00   88
 56  \w     39.00  92.00   0.50   50.00    --  109.75 -95.00 -30.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22597
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.749
_diffrn_reflns_theta_min         4.899
_exptl_absorpt_coefficient_mu    2.062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       needle
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.786
_refine_diff_density_min         -1.370
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.1162
_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^)+28.5069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2165
_refine_ls_wR_factor_ref         0.2245
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2224
_reflns_number_total             2571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00479e2.cif
_cod_data_source_block           2023ncs0480s
_cod_depositor_comments
'Adding full bibliography for 7249127--7249130.cif.'
_cod_database_code               7249129
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.671
_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
 At 1.5 times of:
  All O(H) groups
2. Rigid body (RIGU) restrains
 C4B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: C3B(0.6) H3B(0.6) C4B(0.6) H4B(0.6) C4C(0.4) H4C(0.4) C3C(0.4)
 H3C(0.4)
4.a Secondary CH2 refined with riding coordinates:
 C1B(H1BA,H1BB)
4.b Aromatic/amide H refined with riding coordinates:
 C3B(H3B), C4B(H4B), C6B(H6B), C7B(H7B), C4A(H4A), C5A(H5A), C4C(H4C), C3C(H3C)
4.c X=CH2 refined with riding coordinates:
 N1A(H1AA,H1AB), N2A(H2AA,H2AB)
4.d Idealised tetrahedral OH refined as rotating group:
 O3B(H3BA)
;
_shelx_res_checksum              81219
_shelx_hkl_checksum              41263
_shelx_fab_checksum              68114
_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
- Detector area scaling
;