Nicotinic acid bromide: a simple organic salt optical-electrical ferroelastic with high <i>T</i><sub>c</sub>.
Li, Jie; Zhang, Tie; Lun, Meng-Meng; Su, Chang-Yuan; Zhang, Zhi-Xu; Huang, Pei-Zhi; Zhang, Yi; Teri, Gele; Fu, Da-Wei; Chemical communications (Cambridge, England) 59 (2023) 4644–4647; doi:10.1039/d3cc00776f

data_7131467
_publ_section_title
;
 Nicotinic acid bromide: a simple organic salt optical-electrical
 ferroelastic with high <i>T</i><sub>c</sub>.
;
_journal_issue                   31
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4644
_journal_page_last               4647
_journal_paper_doi               10.1039/d3cc00776f
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'Br, C6 H6 N O2'
_chemical_formula_sum            'C6 H6 Br N O2'
_chemical_formula_weight         204.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-03-21 deposited with the CCDC.	2023-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                79.944(7)
_cell_angle_beta                 86.365(7)
_cell_angle_gamma                68.488(8)
_cell_formula_units_Z            2
_cell_length_a                   7.0700(7)
_cell_length_b                   7.4103(6)
_cell_length_c                   7.5264(7)
_cell_measurement_reflns_used    4031
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5760
_cell_measurement_theta_min      2.7610
_cell_volume                     361.21(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_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    -46.00  16.00   0.50    0.50    --    4.98 -38.00 120.00  124
  2  \w    -18.00  28.00   0.50    0.50    --    4.98 -78.00  89.00   92
  3  \w    -15.00  30.00   0.50    0.50    --    4.98 -99.00   0.00   90
  4  \w     12.00  42.00   0.50    0.50    --    4.98  78.00-145.00   60
  5  \w    -61.00  18.00   0.50    0.50    --    4.98 -38.00   0.00  158
  6  \w    -69.00  17.00   0.50    0.50    --    4.98 -19.00  60.00  172
  7  \w     -8.00  48.00   0.50    0.50    --    4.98  19.00 150.00  112
  8  \w    -34.00  16.00   0.50    0.50    --   -5.77 -78.00  89.00  100
  9  \w    -75.00   5.00   0.50    0.50    --   -5.77 -38.00 -90.00  160
 10  \w    -18.00  10.00   0.50    0.50    --   -5.77  38.00-150.00   56
 11  \w     16.00  67.00   0.50    0.50    --   -5.77  38.00-150.00  102
 12  \w    -29.00  43.00   0.50    0.50    --   -5.77  78.00-145.00  144
 13  \w    -19.00  54.00   0.50    0.50    --   -5.77  38.00 -60.00  146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0720808000
_diffrn_orient_matrix_UB_12      -0.0077607000
_diffrn_orient_matrix_UB_13      -0.0709783000
_diffrn_orient_matrix_UB_21      0.0537827000
_diffrn_orient_matrix_UB_22      -0.0993283000
_diffrn_orient_matrix_UB_23      0.0379747000
_diffrn_orient_matrix_UB_31      -0.0595022000
_diffrn_orient_matrix_UB_32      -0.0307872000
_diffrn_orient_matrix_UB_33      -0.0517768000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8083
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_min         2.749
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.624
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
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    1.876
_exptl_crystal_description       block
_exptl_crystal_F_000             200
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.236
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0902
_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^)+(0.0174P)^2^+7.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1692
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1474
_reflns_number_total             1695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00776f3.cif
_cod_data_source_block           n_b_q_auto_r
_cod_depositor_comments
;
Adding full bibliography for 7131465--7131468.cif.

2025-03-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C12 H12 Br2 N2 O4'
_cod_original_formula_weight         408.06
_cod_original_formula_moiety         '2(Br), 2(C6 H6 N O2)'
_cod_original_formula_units_Z            1
_cod_database_code               7131467
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C1 H1 N1 O1 Br1'
_shelx_estimated_absorpt_t_max   0.603
_shelx_estimated_absorpt_t_min   0.603
_reflns_odcompleteness_completeness 98.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1A), C1(H1B), C2(H2), C3(H3), C5(H5)
2.b Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              30500
_shelx_hkl_checksum              10361
_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 1.944
_oxdiff_exptl_absorpt_empirical_full_min 0.612