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_1572335
_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_absolute_configuration ad
_chemical_formula_moiety         'C42 H45 Br3 N6, 1.5(H2 O), 0.786(O)'
_chemical_formula_sum            'C42 H48 Br3 N6 O2.29'
_chemical_formula_weight         913.15
_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   mixed
_audit_creation_date             2023-01-26
_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                 102.547(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5590(4)
_cell_length_b                   23.3781(6)
_cell_length_c                   16.2798(5)
_cell_measurement_reflns_used    16908
_cell_measurement_temperature    100.01(13)
_cell_measurement_theta_max      25.0480
_cell_measurement_theta_min      1.5380
_cell_volume                     4665.7(2)
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -34.00  -8.00   1.00   50.00    --   -8.70  66.00 163.00   26
  2  \w    -70.00  14.00   1.00   50.00    --   -8.70 -66.00  28.00   84
  3  \w    -45.00  17.00   1.00   50.00    --   -8.70 -38.00  30.00   62
  4  \w    -80.00  19.00   1.00   50.00    --   -8.70 -57.00-120.00   99
  5  \w    -46.00  58.00   1.00   50.00    --   -8.70  68.00-150.00  104
  6  \w     18.00  68.00   1.00   50.00    --   -8.70  66.00 163.00   50
;
_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      0.0144307000
_diffrn_orient_matrix_UB_12      0.0022981000
_diffrn_orient_matrix_UB_13      0.0444928000
_diffrn_orient_matrix_UB_21      0.0376460000
_diffrn_orient_matrix_UB_22      -0.0228001000
_diffrn_orient_matrix_UB_23      0.0015958000
_diffrn_orient_matrix_UB_31      0.0415063000
_diffrn_orient_matrix_UB_32      0.0198682000
_diffrn_orient_matrix_UB_33      -0.0033829000
_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  0.0402
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            55071
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.422
_diffrn_reflns_theta_min         1.549
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku 007HF (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.632
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79637
_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            'dull colourless'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       needle
_exptl_crystal_F_000             1861
_exptl_crystal_preparation
'Slow vapour diffusion of n-heptane into a THF solution.'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.661
_refine_diff_density_min         -1.411
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 5735 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     975
_refine_ls_number_reflns         18957
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+2.6105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1406
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                14728
_reflns_number_total             18957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04207g2.cif
_cod_data_source_block           33-rr_h2o_w0154_sq_ams502_thfhept_100k_1
_cod_depositor_comments
'Adding full bibliography for 1572326--1572335.cif.'
_cod_database_code               1572335
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H45 N6 Br3'
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.663
_reflns_odcompleteness_completeness 99.92
_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 O(H,H) groups
2.a Free rotating group:
 O103(H10C,H10D), O104(H10E,H10F), O106(H10G,H10H)
2.b Ternary CH refined with riding coordinates:
 C79(H79), C10(H10), C28(H28), C78(H78), C11(H11), C44(H44), C95(H95),
 C96(H96), C45(H45), C27(H27), C62(H62), C61(H61)
2.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C14(H14A,H14B), C97(H97A,H97B), C15(H15A,H15B), C83(H83A,
 H83B), C46(H46A,H46B), C13(H13A,H13B), C100(H10A,H10B), C99(H99A,H99B),
 C98(H98A,H98B), C29(H29A,H29B), C47(H47A,H47B), C48(H48A,H48B), C63(H63A,H63B),
  C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C82(H82A,H82B), C80(H80A,
 H80B), C49(H49A,H49B), C66(H66A,H66B), C64(H64A,H64B), C65(H65A,H65B),
 C81(H81A,H81B)
2.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C93(H93), C42(H42), C39(H39), C17(H17), C3(H3), C51(H51),
 C92(H92), C90(H90), C76(H76), C71(H71), C5(H5), C24(H24), C88(H88), C85(H85),
 C34(H34), C56(H56), C22(H22), C73(H73), C20(H20), C59(H59), C68(H68), C75(H75),
  C41(H41), C37(H37), C25(H25), C102(H102), C58(H58), C54(H54)
;
_shelx_res_checksum              52597
_shelx_hkl_checksum              90642
_shelx_fab_checksum              84437
_olex2_date_sample_data_collection 2022-06-08
_olex2_submission_original_sample_id 'AMS502 THF nHept 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 1.132
_oxdiff_exptl_absorpt_empirical_full_min 0.885