New hybrid: [H-β-(4-pyridyl)-Ala-OH] tetrafluoroborate – crystal structure and strong piezoelectricity
Wojtaś, Maciej; Bednarchuk, Tamara J.; Bdikin, Igor; CrystEngComm 25 (2023) 3609–3617; doi:10.1039/D3CE00308F

data_7246805
_publ_section_title
;
 New hybrid: [H-\b-(4-pyridyl)-Ala-OH] tetrafluoroborate -- crystal
 structure and strong piezoelectricity
;
_journal_issue                   25
_journal_name_full               CrystEngComm
_journal_page_first              3609
_journal_page_last               3617
_journal_paper_doi               10.1039/D3CE00308F
_journal_volume                  25
_journal_year                    2023
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C8 H11 N2 O2, B F4'
_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
_audit_creation_date             2022-03-29
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2023-03-10 deposited with the CCDC.	2023-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.79(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.355(3)
_cell_length_b                   8.831(3)
_cell_length_c                   11.415(4)
_cell_measurement_reflns_used    4141
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.6360
_cell_measurement_theta_min      2.8950
_cell_volume                     539.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -25.00  57.00   1.00   20.00    --   13.31 -99.00-120.00   82
  2  \w    -78.00 -32.00   1.00   20.00    --   13.31 178.00 120.00   46
  3  \w    -92.00  18.00   1.00   20.00    --  -14.40 -57.00 -30.00  110
  4  \w    -94.00  17.00   1.00   20.00    --  -14.40 -37.00  60.00  111
  5  \w    -98.00  22.00   1.00   20.00    --  -14.40 -77.00-150.00  120
  6  \w    -47.00  64.00   1.00   20.00    --  -14.40  57.00 120.00  111
  7  \w    -55.00  34.00   1.00   20.00    --  -14.40  91.00 -84.35   89
  8  \w    -25.00  57.00   1.00   20.00    --   13.31 -99.00 120.00   82
  9  \w    -78.00 -33.00   1.00   20.00    --   13.31 178.00-180.00   45
 10  \w     39.00  50.00   1.00   20.00    --   13.31-142.00  82.00   11
 11  \w    -21.00  33.00   1.00   20.00    --  -14.40  92.00 109.36   54
 12  \w    -79.00 -34.00   1.00   20.00    --   13.31   0.00-120.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10961
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.691
_diffrn_reflns_theta_max         25.691
_diffrn_reflns_theta_min         2.916
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       needle
_exptl_crystal_F_000             260
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 797 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2063
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0577P)^2^+0.3569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1154
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                1909
_reflns_number_total             2063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00308f2.cif
_cod_data_source_block           ala-oh-bf4
_cod_depositor_comments          'Adding full bibliography for 7246805.cif.'
_cod_database_code               7246805
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.980
_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.a Ternary CH refined with riding coordinates:
 C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
2.c Aromatic/amide H refined with riding coordinates:
 N11(H11), C13(H13), C15(H15), C16(H16), C12(H12)
2.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              92274
_shelx_hkl_checksum              3273
_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
;