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_7249127
_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 H8 O3 P, H2 O'
_chemical_formula_sum            'C7 H10 O4 P'
_chemical_formula_weight         189.12
_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   mixed
_atom_sites_solution_primary     dual
_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                 93.663(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8893(5)
_cell_length_b                   6.2149(2)
_cell_length_c                   9.0927(3)
_cell_measurement_reflns_used    4129
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.6780
_cell_measurement_theta_min      2.9520
_cell_volume                     839.68(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_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 0.996
_diffrn_measured_fraction_theta_max 0.929
_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   -122.00 -39.00   0.50    1.73    --  -49.15 -16.00 -13.00  166
  2  \w    -33.00  25.00   0.50    1.73    --  -49.15  16.00 155.00  116
  3  \w    -24.00  25.00   0.50    1.73    --   49.15 -16.00 -13.00   98
  4  \w     39.00 123.00   0.50    1.73    --   49.15  16.00 155.00  168
  5  \w   -163.00 -80.00   0.50    6.91    --  -90.00 -16.00 -13.00  166
  6  \w    100.00 178.00   0.50    6.91    --  110.16  16.00 155.00  156
  7  \w   -120.00 -94.00   0.50    1.73    --  -49.15 -57.00 -90.00   52
  8  \w    -23.00  40.00   0.50    1.73    --   49.15 -38.00-120.00  126
  9  \w    -48.00 -18.00   0.50    6.91    --  -90.00  38.00 -90.00   60
 10  \w    -48.00 -18.00   0.50    6.91    --  -90.00  38.00  90.00   60
 11  \w    -48.00 -18.00   0.50    6.91    --  -90.00  38.00 120.00   60
 12  \w    -48.00 -18.00   0.50    6.91    --  -90.00  38.00 -60.00   60
 13  \w    -48.00 -18.00   0.50    6.91    --  -90.00  38.00-120.00   60
 14  \w    -48.00 -18.00   0.50    6.91    --  -90.00  38.00 150.00   60
 15  \w    -69.00 -18.00   0.50    6.91    --  -90.00  57.00 150.00  102
 16  \w    -85.00 -18.00   0.50    6.91    --  -90.00 125.00-150.00  134
 17  \w    -69.00 -18.00   0.50    6.91    --  -90.00  57.00-150.00  102
 18  \w    -69.00 -18.00   0.50    6.91    --  -90.00  57.00 -30.00  102
 19  \w     38.00  97.00   0.50    6.91    --  110.16 -77.00-120.00  118
 20  \w     38.00 112.00   0.50    6.91    --  110.16-125.00-120.00  148
 21  \w     96.00 178.00   0.50    6.91    --  110.16  57.00-150.00  164
 22  \w     38.00 105.00   0.50    6.91    --  110.16 -99.00-180.00  134
 23  \w   -121.00 -38.00   0.50    1.73    --  -49.15 -38.00 -90.00  166
 24  \w   -121.00 -61.00   0.50    1.73    --  -49.15 -38.00  60.00  120
 25  \w     39.00 121.00   0.50    1.73    --   49.15  38.00-150.00  164
;
_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      -0.0986348000
_diffrn_orient_matrix_UB_12      0.0179087000
_diffrn_orient_matrix_UB_13      -0.0614545000
_diffrn_orient_matrix_UB_21      0.0321007000
_diffrn_orient_matrix_UB_22      0.0497858000
_diffrn_orient_matrix_UB_23      -0.1540685000
_diffrn_orient_matrix_UB_31      -0.0002873000
_diffrn_orient_matrix_UB_32      -0.2421029000
_diffrn_orient_matrix_UB_33      -0.0360519000
_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  0.0586
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7416
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.976
_diffrn_reflns_theta_min         2.974
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.730
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.683
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       plate
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0803P)^2^+0.6445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1484
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1458
_reflns_number_total             1664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00479e2.cif
_cod_data_source_block           pi-p_repro
_cod_depositor_comments
'Adding full bibliography for 7249127--7249130.cif.'
_cod_database_code               7249127
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C44  H40  N4  O4  P1  '
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.718
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O1S(H1SA,H1SB)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C6(H6), C7(H7)
2.d Idealised tetrahedral OH refined as rotating group:
 O2(H2), O3(H3)
;
_shelx_res_checksum              97624
_shelx_hkl_checksum              70704
_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 2.327
_oxdiff_exptl_absorpt_empirical_full_min 0.464