Synthesis, structures, and optical properties of N-heterocycle and amino acid ester-coordinated B<sub>3</sub>H<sub>7</sub>.
Chen, Xi-Meng; Chi, Jing-Xian; Li, Yin-Yin; Ge, Yi-Wen; Wang, Peng; Wang, Hongju; Jiang, Kai; Ma, Yan-Na; Chen, Xuenian; Chemical communications (Cambridge, England) 61 (2025) 2313–2316; doi:10.1039/d4cc05845c

data_7134122
_publ_section_title
;
 Synthesis, structures, and optical properties of N-heterocycle and amino
 acid ester-coordinated B<sub>3</sub>H<sub>7</sub>.
;
_journal_issue                   11
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2313
_journal_page_last               2316
_journal_paper_doi               10.1039/d4cc05845c
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C9 H13 B3 Br N'
_chemical_formula_sum            'C9 H13 B3 Br N'
_chemical_formula_weight         247.54
_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
_audit_creation_date             2024-12-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-12-25 deposited with the CCDC.	2025-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.063(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0276(2)
_cell_length_b                   14.8744(4)
_cell_length_c                   11.0026(3)
_cell_measurement_reflns_used    2694
_cell_measurement_temperature    293
_cell_measurement_theta_max      71.1560
_cell_measurement_theta_min      5.9480
_cell_volume                     1149.37(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (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 2019/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.00
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_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     -3.00  32.00   1.00    1.00    --  -35.62  80.00 -55.00   35
  2  \w    -64.00 -35.00   1.00    1.00    --  -35.62  80.00 -55.00   29
  3  \w    119.00 174.00   1.00    1.86    --  106.81  80.00 -55.00   55
  4  \w     51.00 119.00   1.00    1.86    --  106.81 -80.00-178.00   68
  5  \w    -76.00 -43.00   1.00    1.00    --  -35.62-178.00   0.00   33
  6  \w   -108.00 -44.00   1.00    1.00    --  -35.62 178.00  30.00   64
  7  \w    -21.00  59.00   1.00    1.00    --   35.62 -80.00-178.00   80
  8  \w    -32.00   3.00   1.00    1.00    --   35.62 -57.00 -90.00   35
  9  \w      8.00  52.00   1.00    1.00    --   35.62 -57.00 -90.00   44
 10  \w     81.00 107.00   1.00    1.00    --   35.62-178.00 150.00   26
 11  \w     73.00 101.00   1.00    1.00    --   35.62 178.00-180.00   28
 12  \w    105.00 173.00   1.00    1.86    --  106.81 111.00 -90.00   68
 13  \w     99.00 125.00   1.00    1.86    --  106.81 -30.00-180.00   26
 14  \w     54.00  97.00   1.00    1.86    --  106.81-111.00 120.00   43
 15  \w     46.00  73.00   1.00    1.86    --  106.81 -30.00-180.00   27
 16  \w     41.00  66.00   1.00    1.86    --  106.81 -30.00-150.00   25
 17  \w     96.00 126.00   1.00    1.86    --  106.81 -30.00-150.00   30
 18  \w     38.00  63.00   1.00    1.86    --  106.81 -45.00-180.00   25
 19  \w    128.00 172.00   1.00    1.86    --  106.81  77.00-150.00   44
 20  \w     97.00 123.00   1.00    1.86    --  106.81 -45.00-180.00   26
 21  \w    110.00 173.00   1.00    1.86    --  106.81 111.00 150.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4457
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.211
_diffrn_reflns_theta_min         5.002
_exptl_absorpt_coefficient_mu    4.495
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
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    1.431
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.770
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2176
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0669P)^2^+0.9787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1282
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1985
_reflns_number_total             2176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05845c2.cif
_cod_data_source_block           20231123-cjxbr_auto
_cod_depositor_comments
'Adding full bibliography for 7134119--7134122.cif.'
_cod_database_code               7134122
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.662
_shelx_estimated_absorpt_t_min   0.662
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H,H) groups, All B(H,H,H) groups, All C(H) groups
2.a Riding coordinates:
 B1(H1A,H1B), B2(H1C,H2A,H2B), B3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9)
;
_shelx_res_checksum              1728
_shelx_hkl_checksum              11404
_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
;