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_7244247
_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         345.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 94.0110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   14.72130(10)
_cell_length_b                   8.57480(10)
_cell_length_c                   23.2614(3)
_cell_measurement_reflns_used    19575
_cell_measurement_temperature    93
_cell_measurement_theta_max      71.9530
_cell_measurement_theta_min      3.4270
_cell_volume                     2929.15(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 1.000
_diffrn_measured_fraction_theta_max 0.992
_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    -89.00  27.00   0.50    0.50    --    0.00 -38.00 120.00  232
  2  \w    -28.00  89.00   0.50    0.50    --    0.00  57.00   0.00  234
  3  \w    -27.00  89.00   0.50    0.50    --    0.00  38.00  90.00  232
  4  \w     64.00 185.00   0.50    0.50    --   95.70  30.00 -30.00  242
  5  \w      6.00 122.00   0.50    0.50    --   95.70 -45.00-150.00  232
  6  \w      6.00 125.00   0.50    0.50    --   95.70 -61.00 150.00  238
  7  \w      6.00 132.00   0.50    0.50    --   95.70 -82.00  60.00  252
  8  \w     64.00 185.00   0.50    0.50    --   95.70  30.00   0.00  242
  9  \w      6.00 125.00   0.50    0.50    --   95.70 -61.00  60.00  238
 10  \w     69.00 185.00   0.50    0.50    --   95.70  45.00-120.00  232
 11  \w     64.00 185.00   0.50    0.50    --   95.70  30.00 -90.00  242
 12  \w    -27.00  89.00   0.50    0.50    --    0.00  38.00 -30.00  232
 13  \w    -28.00  89.00   0.50    0.50    --    0.00  57.00-120.00  234
 14  \w     64.00 151.00   0.50    0.50    --   95.70  30.00 150.00  174
;
_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      -0.0874228000
_diffrn_orient_matrix_UB_12      0.0707150000
_diffrn_orient_matrix_UB_13      0.0218220000
_diffrn_orient_matrix_UB_21      0.0151893000
_diffrn_orient_matrix_UB_22      -0.0934384000
_diffrn_orient_matrix_UB_23      0.0563600000
_diffrn_orient_matrix_UB_31      0.0558221000
_diffrn_orient_matrix_UB_32      0.1362390000
_diffrn_orient_matrix_UB_33      0.0274622000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            10320
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.360
_diffrn_reflns_theta_min         3.447
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    14.833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22579
_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    2.353
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.667
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.324
_refine_ls_extinction_coef       0.00021(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         10320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0447
_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^)+(0.1144P)^2^+1.4275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1470
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9641
_reflns_number_total             10320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01654g2.cif
_cod_data_source_block           From_TCE
_cod_depositor_comments
;

2025-03-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C2.05 H2.34 Br0.88 N0.29'
_cod_original_formula_weight         101.23
_cod_original_formula_moiety         '0.29(C7 H8 Br2 N), 0.29(Br)'
_cod_original_formula_units_Z            41
_cod_database_code               7244247
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CHNBrCl
_shelx_estimated_absorpt_t_max   0.524
_shelx_estimated_absorpt_t_min   0.155
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5485(11)
 0.4515(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C15(H15A,H15B), C21(H21A,H21B), C14(H14A,H14B), C1(H1A,H1B),
 C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), N2(H2), C4(H4), C20(H20), C17(H17), C13(H13), C6(H6),
 C10(H10), C3(H3A), C11(H11), C18(H18)
;
_shelx_res_checksum              17492
_shelx_hkl_checksum              11784
_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 3.165
_oxdiff_exptl_absorpt_empirical_full_min 0.661