Dynamic and solid-state behaviour of bromoisotrianglimine.
Scholes, Abbie M.; Kershaw Cook, Laurence J.; Szczypiński, Filip T; Luzyanin, Konstantin V.; Egleston, Benjamin D.; Greenaway, Rebecca L.; Slater, Anna G.; Chemical science 15 (2024) 14254–14263; doi:10.1039/d4sc04207g

data_1572326
_publ_section_title
;
 Dynamic and solid-state behaviour of bromoisotrianglimine.
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              14254
_journal_page_last               14263
_journal_paper_doi               10.1039/d4sc04207g
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C28 H30 Br2 N4'
_chemical_formula_sum            'C28 H30 Br2 N4'
_chemical_formula_weight         582.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-11-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-12-07 deposited with the CCDC.	2024-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                99.016(4)
_cell_angle_beta                 92.137(3)
_cell_angle_gamma                109.139(5)
_cell_formula_units_Z            1
_cell_length_a                   6.4446(2)
_cell_length_b                   8.9992(6)
_cell_length_c                   11.3593(4)
_cell_measurement_reflns_used    9089
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.5460
_cell_measurement_theta_min      1.8090
_cell_volume                     611.91(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.889
_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   -101.00   9.00   1.00   10.00    --  -15.10 -57.00-120.00  110
  2  \w    -52.00  11.00   1.00   10.00    --  -15.10  57.00 -30.00   63
  3  \w   -100.00   2.00   1.00   10.00    --  -15.10 -57.00   0.00  102
  4  \w    -53.00  17.00   1.00   10.00    --  -15.10  57.00  90.00   70
  5  \w    -55.00 -24.00   1.00   10.00    --  -15.10  68.00-150.00   31
  6  \w    -21.00  27.00   1.00   10.00    --  -15.10  68.00-150.00   48
  7  \w     44.00  74.00   1.00   10.00    --  -15.10  68.00-150.00   30
  8  \w   -103.00 -19.00   1.00   10.00    --  -15.10 -19.00 120.00   84
  9  \w     17.00  74.00   1.00   10.00    --  -15.10 -19.00 120.00   57
 10  \w    -51.00 -22.00   1.00   10.00    --  -15.10  68.00   0.00   29
 11  \w    -18.00   9.00   1.00   10.00    --  -15.10  68.00   0.00   27
 12  \w    -44.00  66.00   1.00   10.00    --  -15.10  57.00-180.00  110
 13  \w    -93.00  24.00   1.00   10.00    --  -15.10 -68.00 120.00  117
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0358272000
_diffrn_orient_matrix_UB_12      -0.0847366000
_diffrn_orient_matrix_UB_13      -0.0101614000
_diffrn_orient_matrix_UB_21      0.0328289000
_diffrn_orient_matrix_UB_22      -0.0005869000
_diffrn_orient_matrix_UB_23      -0.0589321000
_diffrn_orient_matrix_UB_31      0.1064650000
_diffrn_orient_matrix_UB_32      0.0031833000
_diffrn_orient_matrix_UB_33      0.0213871000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3047
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.557
_diffrn_reflns_theta_min         1.823
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku 007HF (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.337
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       plank
_exptl_crystal_F_000             296
_exptl_crystal_preparation
;
Slow vapour diffusion of 1,4-dioxane into a dichloromethane solution of a 1:1 stoichiometric ratio of the RR- and SS- enantiomers
containing a mixture of the [3+3] and [2+2] macrocyclic forms.
;
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+2.8160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2901
_reflns_number_total             3047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04207g2.cif
_cod_data_source_block           22-meso_v0318_tw_ams371-3_dcmdiox_100k_plank_1
_cod_depositor_comments
'Adding full bibliography for 1572326--1572335.cif.'
_cod_database_code               1572326
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C28 H30 Br2 N4'
_shelx_estimated_absorpt_t_max   0.851
_shelx_estimated_absorpt_t_min   0.424
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.729(3)
 0.271(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Ternary CH refined with riding coordinates:
 C11(H11), C10(H10)
3.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C12(H12A,H12B), C14(H14A,H14B), C13(H13A,H13B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C17(H17), C7(H7)
;
_shelx_res_checksum              84604
_shelx_hkl_checksum              2894
_olex2_date_sample_data_collection 2022-02-11
_olex2_submission_original_sample_id 'AMS371-3 DCMDiox Plank 100 K'
_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 1.332
_oxdiff_exptl_absorpt_empirical_full_min 0.766