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_7244226
_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         'C7 H8 Br2 N, Br'
_chemical_formula_sum            'C7 H8 Br3 N'
_chemical_formula_weight         345.87
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                   8.12360(10)
_cell_length_b                   14.0468(2)
_cell_length_c                   16.9496(3)
_cell_measurement_reflns_used    4183
_cell_measurement_temperature    93
_cell_measurement_theta_max      71.9070
_cell_measurement_theta_min      6.7860
_cell_volume                     1934.13(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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      93
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.975
_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   2.00   0.50    0.50    --    0.00  82.00-120.00   54
  2  \w    -60.00 -21.00   0.50    0.50    --    0.00 -38.00 -90.00   78
  3  \w    -12.00  27.00   0.50    0.50    --    0.00 -38.00 -90.00   78
  4  \w     41.00  88.00   0.50    0.50    --    0.00  82.00-120.00   94
  5  \w     16.00 106.00   0.50    0.50    --   95.70 -82.00  60.00  180
  6  \w     27.00 113.00   0.50    0.50    --   95.70 -45.00-150.00  172
  7  \w     83.00 126.00   0.50    0.50    --   95.70 -82.00 -30.00   86
  8  \w     90.00 126.00   0.50    0.50    --   95.70 -77.00  30.00   72
  9  \w     19.00 122.00   0.50    0.50    --   95.70 -15.00  90.00  206
;
_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      0.1305261000
_diffrn_orient_matrix_UB_12      -0.0041612000
_diffrn_orient_matrix_UB_13      0.0657524000
_diffrn_orient_matrix_UB_21      0.1377412000
_diffrn_orient_matrix_UB_22      0.0061127000
_diffrn_orient_matrix_UB_23      -0.0624234000
_diffrn_orient_matrix_UB_31      -0.0023621000
_diffrn_orient_matrix_UB_32      0.1093785000
_diffrn_orient_matrix_UB_33      0.0060027000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5588
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.041
_diffrn_reflns_theta_min         5.219
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    14.976
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
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    2.376
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.968
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0595P)^2^+4.8665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0967
_refine_ls_wR_factor_ref         0.0980
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1748
_reflns_number_total             1849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01654g2.cif
_cod_data_source_block           From_MeCN
_cod_database_code               7244226
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CHN
_shelx_estimated_absorpt_t_max   0.467
_shelx_estimated_absorpt_t_min   0.137
_reflns_odcompleteness_completeness 99.55
_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.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C4(H4), C3(H3), C6(H6)
;
_shelx_res_checksum              17499
_shelx_hkl_checksum              47245
_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 1.650
_oxdiff_exptl_absorpt_empirical_full_min 0.635