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_1572332
_publ_section_title
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 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_absolute_configuration ad
_chemical_formula_moiety         'C42 H45 Br3 N6, 1.262(C H4 O)'
_chemical_formula_sum            'C43.26 H50.05 Br3 N6 O1.26'
_chemical_formula_weight         914.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-11-16
_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                 92.298(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8142(3)
_cell_length_b                   19.7153(4)
_cell_length_c                   14.9459(3)
_cell_measurement_reflns_used    22494
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      25.0750
_cell_measurement_theta_min      2.1690
_cell_volume                     4361.68(15)
_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      150.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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    -44.00  80.00   1.00  150.00    --   -8.90  54.00 166.00  124
  2  \w    -98.00 -10.00   1.00  150.00    --   -8.90 -54.00  22.00   88
  3  \w    -45.00  80.00   1.00  150.00    --   -8.90  68.00 -90.00  125
  4  \w    -97.00  -3.00   1.00  150.00    --   -8.90 -68.00  90.00   94
  5  \w    -73.00 -48.00   1.00  150.00    --   -8.90 -57.00-150.00   25
  6  \w     -5.00  25.00   1.00  150.00    --   -8.90 -57.00-150.00   30
  7  \w    -96.00  25.00   1.00  150.00    --   -8.90 -57.00 -60.00  121
;
_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      -0.0478683000
_diffrn_orient_matrix_UB_12      0.0017795000
_diffrn_orient_matrix_UB_13      -0.0021641000
_diffrn_orient_matrix_UB_21      -0.0017476000
_diffrn_orient_matrix_UB_22      -0.0231604000
_diffrn_orient_matrix_UB_23      0.0362334000
_diffrn_orient_matrix_UB_31      0.0016546000
_diffrn_orient_matrix_UB_32      0.0274595000
_diffrn_orient_matrix_UB_33      0.0306369000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            73302
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_min         2.161
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku 007HF (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.814
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77423
_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    1.392
_exptl_crystal_description       plate
_exptl_crystal_F_000             1867
_exptl_crystal_preparation       'Slow evaporation of a methanol solution.'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.978
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 5463 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     982
_refine_ls_number_reflns         19721
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0610P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1090
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                14387
_reflns_number_total             19721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04207g2.cif
_cod_data_source_block           33-ss_meoh_x0038_ams649_meoh_150k_1_bsme
_cod_depositor_comments
'Adding full bibliography for 1572326--1572335.cif.'
_cod_database_code               1572332
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C43 H50 N6 O Br3'
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.631
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All O(H) groups
2. Others
 Sof(O105)=Sof(H105)=Sof(C106)=Sof(H10I)=Sof(H10J)=Sof(H10K)=FVAR(1)
 Sof(O107)=Sof(H107)=Sof(C108)=Sof(H10F)=Sof(H10G)=Sof(H10H)=FVAR(2)
 Sof(O103)=Sof(H103)=Sof(C104)=Sof(H10C)=Sof(H10D)=Sof(H10E)=FVAR(3)
3.a Ternary CH refined with riding coordinates:
 C44(H44), C96(H96), C45(H45), C28(H28), C78(H78), C27(H27), C95(H95),
 C11(H11), C10(H10), C79(H79), C62(H62), C61(H61)
3.b Secondary CH2 refined with riding coordinates:
 C97(H97A,H97B), C98(H98A,H98B), C80(H80A,H80B), C47(H47A,H47B), C48(H48A,
 H48B), C81(H81A,H81B), C99(H99A,H99B), C49(H49A,H49B), C100(H10A,H10B),
 C32(H32A,H32B), C83(H83A,H83B), C82(H82A,H82B), C15(H15A,H15B), C46(H46A,H46B),
  C12(H12A,H12B), C29(H29A,H29B), C65(H65A,H65B), C14(H14A,H14B), C30(H30A,
 H30B), C31(H31A,H31B), C13(H13A,H13B), C63(H63A,H63B), C64(H64A,H64B),
 C66(H66A,H66B)
3.c Aromatic/amide H refined with riding coordinates:
 C51(H51), C37(H37), C76(H76), C68(H68), C42(H42), C71(H71), C102(H102),
 C58(H58), C75(H75), C41(H41), C25(H25), C24(H24), C88(H88), C22(H22), C59(H59),
  C92(H92), C5(H5), C85(H85), C34(H34), C93(H93), C3(H3), C8(H8), C20(H20),
 C56(H56), C90(H90), C17(H17), C54(H54), C73(H73), C39(H39), C7(H7)
3.d Idealised Me refined as rotating group:
 C104(H10C,H10D,H10E), C106(H10I,H10J,H10K), C108(H10F,H10G,H10H)
3.e Idealised tetrahedral OH refined as rotating group:
 O103(H103), O107(H107), O105(H105)
;
_shelx_res_checksum              76437
_shelx_hkl_checksum              37902
_olex2_date_sample_data_collection 2022-09-23
_olex2_submission_original_sample_id 'AMS649 SS33 MeOH 150 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 1.282
_oxdiff_exptl_absorpt_empirical_full_min 0.809