Pnictogen bonding in imide derivatives for chiral folding and self-assembly.
Wang, Zhuoer; Cao, Zhaozhen; Hao, Aiyou; Xing, Pengyao; Chemical science 15 (2024) 6924–6933; doi:10.1039/d4sc00554f

data_1571405
_publ_section_title
;
 Pnictogen bonding in imide derivatives for chiral folding and
 self-assembly.
;
_journal_issue                   18
_journal_name_full               'Chemical science'
_journal_page_first              6924
_journal_page_last               6933
_journal_paper_doi               10.1039/d4sc00554f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C15 H11 Br0.969 N O3'
_chemical_formula_sum            'C15 H11 Br0.97 N O3'
_chemical_formula_weight         330.76
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2023-11-22 deposited with the CCDC.	2024-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.798(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3573(4)
_cell_length_b                   8.0361(6)
_cell_length_c                   21.7154(13)
_cell_measurement_reflns_used    2923
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      29.8790
_cell_measurement_theta_min      2.8010
_cell_volume                     1281.08(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.816
_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    -23.00  30.00   1.00    2.80    --   -7.76 -99.00 -30.00   53
  2  \w    -11.00  14.00   1.00    2.80    --   -7.76-102.00-130.00   25
  3  \w     -7.00  18.00   1.00    2.80    --    8.78-102.00-130.00   25
  4  \w    -22.00  46.00   1.00    2.80    --    8.78 -99.00-180.00   68
  5  \w    -26.00  66.00   1.00    2.80    --   -7.76  57.00 -90.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0090307000
_diffrn_orient_matrix_UB_12      -0.0161129000
_diffrn_orient_matrix_UB_13      -0.0321675000
_diffrn_orient_matrix_UB_21      -0.0306926000
_diffrn_orient_matrix_UB_22      0.0826755000
_diffrn_orient_matrix_UB_23      -0.0054228000
_diffrn_orient_matrix_UB_31      0.0912102000
_diffrn_orient_matrix_UB_32      0.0262188000
_diffrn_orient_matrix_UB_33      -0.0027475000
_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  0.0529
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.816
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9663
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.325
_diffrn_reflns_theta_min         2.775
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.121
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (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    1.715
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0542
_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^)+2.8422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2358
_reflns_number_total             3148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc00554f2.cif
_cod_data_source_block           c32_auto
_cod_depositor_comments
'Adding full bibliography for 1571402--1571406.cif.'
_cod_database_code               1571405
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.835
_reflns_odcompleteness_completeness 98.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C15(H15), C8(H8), C14(H14)
2.c Idealised tetrahedral OH refined as rotating group:
 O19(H19)
;
_shelx_res_checksum              51963
_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 1.316
_oxdiff_exptl_absorpt_empirical_full_min 0.566