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_7249128
_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         'C18 H18 N O5 P'
_chemical_formula_sum            'C18 H18 N O5 P'
_chemical_formula_weight         359.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 97.9423(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.51236(3)
_cell_length_b                   15.23409(8)
_cell_length_c                   19.29148(11)
_cell_measurement_reflns_used    23833
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.4910
_cell_measurement_theta_min      2.8920
_cell_volume                     1604.478(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.944
_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 -55.00   0.50    1.00    --  -47.67-152.00 -46.00  128
  2  \w    -84.00 -11.00   0.50    1.00    --  -47.67 122.00-165.00  146
  3  \w     32.00  93.00   0.50    1.00    --   47.67-122.00 113.00  122
  4  \w     48.00 111.00   0.50    1.00    --   47.67-152.00 -46.00  126
  5  \w   -147.00 -55.00   0.50    4.00    --  -90.00-152.00 -46.00  184
  6  \w   -161.00 -75.00   0.50    4.00    --  -90.00-122.00 113.00  172
  7  \w     48.00 130.00   0.50    4.00    --  110.64-152.00 -46.00  164
  8  \w     97.00 178.00   0.50    4.00    --  110.64 122.00-165.00  162
  9  \w     40.00 110.00   0.50    4.00    --  110.64-122.00 113.00  140
 10  \w    -34.00  27.00   0.50    1.00    --  -47.67  19.00  60.00  122
 11  \w    -34.00  27.00   0.50    1.00    --  -47.67  19.00 150.00  122
 12  \w    -24.00  40.00   0.50    1.00    --   47.67 -38.00-150.00  128
 13  \w    -48.00 -18.00   0.50    4.00    --  -90.00  38.00-120.00   60
 14  \w    -48.00 -18.00   0.50    4.00    --  -90.00  38.00-150.00   60
 15  \w    -48.00 -18.00   0.50    4.00    --  -90.00  38.00  60.00   60
 16  \w    -69.00 -18.00   0.50    4.00    --  -90.00  57.00-180.00  102
 17  \w    -48.00 -18.00   0.50    4.00    --  -90.00  38.00  30.00   60
 18  \w   -161.00 -94.00   0.50    4.00    --  -90.00 -57.00 120.00  134
 19  \w   -161.00-102.00   0.50    4.00    --  -90.00 -99.00 -30.00  118
 20  \w    -48.00 -18.00   0.50    4.00    --  -90.00  38.00 -30.00   60
 21  \w    -69.00 -18.00   0.50    4.00    --  -90.00  57.00-150.00  102
 22  \w   -161.00-105.00   0.50    4.00    --  -90.00 -77.00-150.00  112
 23  \w    -48.00 -18.00   0.50    4.00    --  -90.00  38.00   0.00   60
 24  \w     40.00 111.00   0.50    4.00    --  110.64-125.00-120.00  142
 25  \w     40.00 106.00   0.50    4.00    --  110.64 -99.00 150.00  132
 26  \w     40.00 106.00   0.50    4.00    --  110.64 -99.00 120.00  132
 27  \w   -120.00 -38.00   0.50    1.00    --  -47.67 -38.00 -60.00  164
 28  \w   -120.00 -38.00   0.50    1.00    --  -47.67 -38.00-120.00  164
 29  \w   -120.00 -38.00   0.50    1.00    --  -47.67 -38.00   0.00  164
 30  \w   -120.00 -38.00   0.50    1.00    --  -47.67 -38.00  60.00  164
 31  \w   -120.00 -38.00   0.50    1.00    --  -47.67 -38.00-180.00  164
 32  \w   -120.00 -38.00   0.50    1.00    --  -47.67 -38.00 -30.00  164
 33  \w   -120.00 -38.00   0.50    1.00    --  -47.67 -38.00 120.00  164
 34  \w   -162.00 -83.00   0.50    4.00    --  -90.00 -38.00  30.00  158
 35  \w   -162.00 -79.00   0.50    4.00    --  -90.00 -38.00 150.00  166
 36  \w   -162.00 -79.00   0.50    4.00    --  -90.00 -38.00 -30.00  166
 37  \w     40.00 106.00   0.50    4.00    --  110.64 -99.00 -30.00  132
;
_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  0.0191
_diffrn_reflns_av_unetI/netI     0.0077
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27458
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.688
_diffrn_reflns_theta_min         3.711
_exptl_absorpt_coefficient_mu    1.796
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
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    1.487
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0424P)^2^+0.9588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3216
_reflns_number_total             3248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00479e2.cif
_cod_data_source_block           aa_ndi_3_repro
_cod_depositor_comments
'Adding full bibliography for 7249127--7249130.cif.'
_cod_original_cell_volume        1604.478(16)
_cod_database_code               7249128
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.433
_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 C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C10(H10), C11(H11), C15(H15), C16(H16)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              96689
_shelx_hkl_checksum              32127
_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
;