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_1572327
_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         'C42 H45 Br3 N6, 0.699(C3 H7)'
_chemical_formula_sum            'C44.1 H49.89 Br3 N6'
_chemical_formula_weight         903.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-11-11
_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                90
_cell_angle_beta                 101.598(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.6941(11)
_cell_length_b                   14.3036(7)
_cell_length_c                   27.0164(13)
_cell_measurement_reflns_used    8883
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      24.5220
_cell_measurement_theta_min      1.5510
_cell_volume                     8969.2(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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 2018/2 (Sheldrick, 2018)'
_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 0.996
_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   -104.00  25.00   1.00  100.00    --  -15.10 -68.00-180.00  129
  2  \w    -55.00  74.00   1.00  100.00    --  -15.10  68.00 150.00  129
  3  \w    -92.00   3.00   1.00  100.00    --  -15.10 -68.00 120.00   95
  4  \w    -41.00  68.00   1.00  100.00    --  -15.10  19.00 -60.00  109
  5  \w    -95.00  -3.00   1.00  100.00    --  -15.10 -68.00  30.00   92
;
_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      0.0016668000
_diffrn_orient_matrix_UB_12      0.0476016000
_diffrn_orient_matrix_UB_13      -0.0069018000
_diffrn_orient_matrix_UB_21      -0.0114279000
_diffrn_orient_matrix_UB_22      -0.0117351000
_diffrn_orient_matrix_UB_23      -0.0255774000
_diffrn_orient_matrix_UB_31      -0.0282853000
_diffrn_orient_matrix_UB_32      0.0074583000
_diffrn_orient_matrix_UB_33      0.0041045000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1108
_diffrn_reflns_av_unetI/netI     0.0985
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            42323
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.389
_diffrn_reflns_theta_min         1.539
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku 007HF (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.734
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
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    1.338
_exptl_crystal_description       block
_exptl_crystal_F_000             3692
_exptl_crystal_preparation
'Slow vapour diffusion of n-hexane into an ethylacetate solution of a 1:1 mixture of the [3+3]-RR and [3+3]-SS bromo substituted macryocycles.'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.589
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8202
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1507
_refine_ls_R_factor_gt           0.0942
_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^)+(0.0883P)^2^+157.7715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2224
_refine_ls_wR_factor_ref         0.2449
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4889
_reflns_number_total             8202
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 6.9391\% 
around [-0.89 -0.14 0.44] (reciprocal) or [-0.89 -0.40 0.20] (direct)
;
_cod_data_source_file            d4sc04207g2.cif
_cod_data_source_block           33-rac_ams330-4_etoachex_100k_v0332_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 1572326--1572335.cif.'
_cod_original_formula_sum        'C44.10 H49.89 Br3 N6'
_cod_database_code               1572327
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Br3 C42 H45 N6'
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.625
_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 C(H,H,H) groups
2. Restrained distances
 C54-C53 = C52-C53
 1.5 with sigma of 0.01
3. Others
 Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C52)=Sof(H52A)=
 Sof(H52B)=Sof(H52C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C11(H11), C45(H45), C28(H28), C10(H10), C27(H27), C44(H44)
4.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C31(H31A,H31B), C12(H12A,H12B), C32(H32A,
 H32B), C48(H48A,H48B), C29(H29A,H29B), C30(H30A,H30B), C47(H47A,H47B),
 C46(H46A,H46B), C14(H14A,H14B), C49(H49A,H49B), C54(H54A,H54B), C53(H53A,H53B)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C34(H34), C39(H39), C17(H17), C8(H8), C20(H20), C24(H24), C3(H3),
 C41(H41), C51(H51), C42(H42), C7(H7), C22(H22), C37(H37), C25(H25)
4.d Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C)
;
_shelx_res_checksum              47575
_shelx_hkl_checksum              19213
_olex2_date_sample_data_collection 2022-02-16
_olex2_submission_original_sample_id 'AMS330-4 EtOAc Hex 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 1.260
_oxdiff_exptl_absorpt_empirical_full_min 0.801
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2