Orientational isomerisation of guest molecules in equilibrium in a tubular host crystal formed via halogen and hydrogen bonding
Yamashita, Yutaro; Tashiro, Shohei; Shionoya, Mitsuhiko; CrystEngComm  (2022) –; doi:10.1039/D1CE01654G

data_7244245
_publ_section_title
;
 Orientational isomerisation of guest molecules in equilibrium in a
 tubular host crystal formed via halogen and hydrogen bonding
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D1CE01654G
_journal_year                    2022
_chemical_formula_moiety         'Br, C7 H8 Br2 N, C0.5 H Br'
_chemical_formula_sum            'C7.5 H9 Br4 N'
_chemical_formula_weight         432.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-11-24
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-26 deposited with the CCDC.	2022-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.5252(4)
_cell_length_b                   11.2799(2)
_cell_length_c                   8.9163(2)
_cell_measurement_reflns_used    4050
_cell_measurement_temperature    148
_cell_measurement_theta_max      71.7050
_cell_measurement_theta_min      3.8400
_cell_volume                     2366.05(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      148
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_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    -54.00  20.00   0.50    0.50    --    0.00 -38.00  60.00  148
  2  \w     10.00  41.00   0.50    0.50    --    0.00  38.00  90.00   62
  3  \w    102.00 131.00   0.50    0.83    --   95.70  45.00-150.00   58
  4  \w     81.00 114.00   0.50    0.83    --   95.70 -82.00 -30.00   66
  5  \w     35.00  73.00   0.50    0.83    --   95.70 -82.00 -30.00   76
  6  \w    134.00 178.00   0.50    0.83    --   95.70  45.00-150.00   88
  7  \w     31.00 130.00   0.50    0.83    --   95.70 -82.00-120.00  198
  8  \w     69.00 103.00   0.50    0.83    --   95.70 -82.00 -90.00   68
  9  \w     64.00 185.00   0.50    0.83    --   95.70  30.00 150.00  242
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0528830000
_diffrn_orient_matrix_UB_12      0.0798973000
_diffrn_orient_matrix_UB_13      -0.0131568000
_diffrn_orient_matrix_UB_21      0.0385642000
_diffrn_orient_matrix_UB_22      0.1102132000
_diffrn_orient_matrix_UB_23      -0.0084339000
_diffrn_orient_matrix_UB_31      0.0021615000
_diffrn_orient_matrix_UB_32      -0.0114192000
_diffrn_orient_matrix_UB_33      -0.1720334000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7415
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.205
_diffrn_reflns_theta_min         3.758
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    16.248
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
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    2.430
_exptl_crystal_description       plate
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.532
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2286
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0762P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2066
_reflns_number_total             2286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01654g2.cif
_cod_data_source_block           DBM_148K
_cod_original_formula_sum        'C7.50 H9 Br4 N'
_cod_database_code               7244245
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CHNBr
_shelx_estimated_absorpt_t_max   0.737
_shelx_estimated_absorpt_t_min   0.085
_diffrn_oxdiff_digest_frames
;
01f9eb994db1eae252530f2466fbb0bdd2000297d92
;
_diffrn_oxdiff_digest_hkl
;
01632695d8434b2ed382ccaab02cdd6b4bd800
;
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Others
 Fixed Sof: H1GA(0.5) H1GB(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1G(H1GA,H1GB), C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C6(H6), C4(H4)
;
_shelx_res_checksum              95339
_shelx_hkl_checksum              48291
_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 4.293
_oxdiff_exptl_absorpt_empirical_full_min 0.323