Crystal structure and piezoelectric properties of the final member of the pyridylalanine derivative series: [H-β-(3-pyridyl)-Ala-OH][BF4]
Wojtaś, Maciej; Gągor, Anna; Bdikin, Igor; Kopyl, Svitlana; CrystEngComm 27 (2025) 6679–6686; doi:10.1039/D5CE00693G

data_7250875
_publ_section_title
;
 Crystal structure and piezoelectric properties of the final member of the
 pyridylalanine derivative series: [H-\b-(3-pyridyl)-Ala-OH][BF4]
;
_journal_issue                   40
_journal_name_full               CrystEngComm
_journal_page_first              6679
_journal_page_last               6686
_journal_paper_doi               10.1039/D5CE00693G
_journal_volume                  27
_journal_year                    2025
_chemical_absolute_configuration unk
_chemical_formula_moiety         'B F4, C8 H11 N2 O2'
_chemical_formula_sum            'C8 H11 B F4 N2 O2'
_chemical_formula_weight         254.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-02-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-05-27 deposited with the CCDC.	2025-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.056(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.0698(8)
_cell_length_b                   14.565(2)
_cell_length_c                   14.099(2)
_cell_measurement_reflns_used    444
_cell_measurement_temperature    85.0(5)
_cell_measurement_theta_max      19.7500
_cell_measurement_theta_min      4.0170
_cell_volume                     1033.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      85.0(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.868
_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     39.00  94.00   1.00  150.00    --   13.67 178.00 120.00   55
  2  \w    -62.00  38.00   1.00  150.00    --   13.67 -57.00 -90.00  100
  3  \w    -35.00 -10.00   1.00  150.00    --  -14.45 -77.00  90.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0097912000
_diffrn_orient_matrix_UB_12      0.0264718000
_diffrn_orient_matrix_UB_13      0.0416798000
_diffrn_orient_matrix_UB_21      -0.0731973000
_diffrn_orient_matrix_UB_22      0.0339227000
_diffrn_orient_matrix_UB_23      -0.0281034000
_diffrn_orient_matrix_UB_31      -0.1200556000
_diffrn_orient_matrix_UB_32      -0.0228369000
_diffrn_orient_matrix_UB_33      0.0064477000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0882
_diffrn_reflns_av_unetI/netI     0.2586
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4639
_diffrn_reflns_point_group_measured_fraction_full 0.731
_diffrn_reflns_point_group_measured_fraction_max 0.605
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.012
_diffrn_reflns_theta_min         2.797
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       plate
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Flack x determined using 318 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -1.2(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         3311
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.2294
_refine_ls_R_factor_gt           0.0944
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0898P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.2424
_reflns_Friedel_coverage         0.345
_reflns_Friedel_fraction_full    0.440
_reflns_Friedel_fraction_max     0.322
_reflns_number_gt                1431
_reflns_number_total             3311
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00693g3.cif
_cod_data_source_block           ala85K
_cod_depositor_comments          'Adding full bibliography for 7250875.cif.'
_cod_database_code               7250875
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C9B) \\sim Ueq, Uanis(C8B) \\sim Ueq, Uanis(C7B) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(O1B) \\sim Ueq, Uanis(O2A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(N2A) \\sim Ueq, Uanis(C5B) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C6B)
\\sim Ueq, Uanis(N1A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C2A) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.001
Uanis(N2B) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(B2)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C8B(H8B), C8A(H8A)
3.b Secondary CH2 refined with riding coordinates:
 C7B(H7BA,H7BB), C7A(H7AA,H7AB)
3.c Aromatic/amide H refined with riding coordinates:
 N1A(H1A), N1B(H1B), C6A(H6A), C5B(H5B), C4A(H4A), C5A(H5A), C2B(H2B),
 C4B(H4B), C6B(H6B), C2A(H2A)
3.d Idealised Me refined as rotating group:
 N2A(H2AA,H2AB,H2AC), N2B(H2BA,H2BB,H2BC)
;
_shelx_res_checksum              42397
_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 1.663
_oxdiff_exptl_absorpt_empirical_full_min 0.633