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_1572334
_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'
_chemical_formula_sum            'C42 H45 Br3 N6'
_chemical_formula_weight         873.57
_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             2022-09-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-12-07 deposited with the CCDC.	2024-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.9080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5723(3)
_cell_length_b                   18.9659(3)
_cell_length_c                   14.9238(2)
_cell_measurement_reflns_used    44387
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      27.7610
_cell_measurement_theta_min      1.7200
_cell_volume                     4122.31(12)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (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 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    -98.00  80.00   1.00    4.00    --   -8.90  23.00-158.00  178
  2  \w    -98.00  26.00   1.00    4.00    --   -8.90 -57.00 -30.00  124
  3  \w    -44.00  80.00   1.00    4.00    --   -8.90  57.00 -60.00  124
  4  \w    -98.00  26.00   1.00    4.00    --   -8.90 -57.00-120.00  124
  5  \w    -46.00  80.00   1.00    4.00    --   -8.90  68.00   0.00  126
  6  \w    -98.00  80.00   1.00    4.00    --   -8.90   0.00-180.00  178
  7  \w    -54.00  80.00   1.00    4.00    --   -8.90  38.00-120.00  134
  8  \w    -98.00  24.00   1.00    4.00    --   -8.90 -68.00-180.00  122
  9  \w    -98.00  26.00   1.00    4.00    --   -8.90 -57.00  90.00  124
;
_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      -0.0481981000
_diffrn_orient_matrix_UB_12      0.0053996000
_diffrn_orient_matrix_UB_13      -0.0011447000
_diffrn_orient_matrix_UB_21      -0.0014500000
_diffrn_orient_matrix_UB_22      -0.0099322000
_diffrn_orient_matrix_UB_23      0.0457806000
_diffrn_orient_matrix_UB_31      0.0068937000
_diffrn_orient_matrix_UB_32      0.0356355000
_diffrn_orient_matrix_UB_33      0.0128463000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_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       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            145655
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.321
_diffrn_reflns_theta_min         1.737
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku 007HF (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.972
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.171
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_preparation
'Slow evaporation of a methanol solution followed by annealing under the cryostream at 375 K for 15 minutes.'
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.126
_refine_diff_density_max         1.198
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.002(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         20267
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0755
_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^)+(0.1138P)^2^+10.3415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.1829
_reflns_Friedel_coverage         0.926
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                17354
_reflns_number_total             20267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04207g2.cif
_cod_data_source_block           33-rr_desolv_w0077_ams337-3_meoh_100k_1
_cod_depositor_comments
'Adding full bibliography for 1572326--1572335.cif.'
_cod_database_code               1572334
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H45 N6 Br3'
_shelx_estimated_absorpt_t_max   0.706
_shelx_estimated_absorpt_t_min   0.400
_reflns_odcompleteness_completeness 99.97
_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
2.a Ternary CH refined with riding coordinates:
 C28(H28), C44(H44), C10(H10), C96(H96), C79(H79), C27(H27), C95(H95),
 C78(H78), C11(H11), C45(H45), C62(H62), C61(H61)
2.b Secondary CH2 refined with riding coordinates:
 C98(H98A,H98B), C13(H13A,H13B), C15(H15A,H15B), C100(H10A,H10B), C99(H99A,
 H99B), C83(H83A,H83B), C97(H97A,H97B), C12(H12A,H12B), C29(H29A,H29B),
 C14(H14A,H14B), C32(H32A,H32B), C81(H81A,H81B), C82(H82A,H82B), C46(H46A,H46B),
  C31(H31A,H31B), C80(H80A,H80B), C30(H30A,H30B), C49(H49A,H49B), C47(H47A,
 H47B), C48(H48A,H48B), C64(H64A,H64B), C63(H63A,H63B), C66(H66A,H66B),
 C65(H65A,H65B)
2.c Aromatic/amide H refined with riding coordinates:
 C102(H102), C17(H17), C8(H8), C24(H24), C90(H90), C76(H76), C93(H93),
 C25(H25), C68(H68), C20(H20), C39(H39), C92(H92), C34(H34), C71(H71), C75(H75),
  C37(H37), C56(H56), C59(H59), C85(H85), C58(H58), C88(H88), C5(H5), C41(H41),
 C51(H51), C22(H22), C42(H42), C54(H54), C7(H7), C73(H73), C3(H3)
;
_shelx_res_checksum              88842
_shelx_hkl_checksum              47488
_olex2_date_sample_data_collection 2022-04-26
_olex2_submission_original_sample_id 'AMS337-1 MeOH Desolv 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 1.712
_oxdiff_exptl_absorpt_empirical_full_min 0.630