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_1572330
_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, 1.25(C1 H4 O1)'
_chemical_formula_sum            'C43.24 H49.97 Br3 N6 O1.25'
_chemical_formula_weight         913.45
_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             2022-09-10
_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                 92.335(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8232(7)
_cell_length_b                   19.6544(10)
_cell_length_c                   14.9442(7)
_cell_measurement_reflns_used    9300
_cell_measurement_temperature    149.99
_cell_measurement_theta_max      26.320
_cell_measurement_theta_min      2.487
_cell_volume                     4350.2(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            66078
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.440
_diffrn_reflns_theta_min         2.481
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.822
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1381 before and 0.0879 after correction. The Ratio of minimum to maximum transmission is 0.7321. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       plate
_exptl_crystal_F_000             1866
_exptl_crystal_preparation       'Slow evaporation of a methanol solution.'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.631
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 5266 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.070(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     982
_refine_ls_number_reflns         17694
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0309P)^2^+9.4181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1204
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                13970
_reflns_number_total             17694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04207g2.cif
_cod_data_source_block           '[3+3]-rr_meoh_ams2a3a_us_150k_1'
_cod_depositor_comments
'Adding full bibliography for 1572326--1572335.cif.'
_cod_database_code               1572330
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.430
_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(O103)=Sof(H103)=Sof(C104)=Sof(H10C)=Sof(H10D)=Sof(H10E)=FVAR(1)
 Sof(O105)=Sof(H105)=Sof(C106)=Sof(H10I)=Sof(H10J)=Sof(H10K)=FVAR(2)
 Sof(O107)=Sof(H107)=Sof(C108)=Sof(H10F)=Sof(H10G)=Sof(H10H)=FVAR(3)
3.a Ternary CH refined with riding coordinates:
 C10(H10), C96(H96), C78(H78), C45(H45), C27(H27), C11(H11), C62(H62),
 C95(H95), C44(H44), C28(H28), C79(H79), C61(H61)
3.b Secondary CH2 refined with riding coordinates:
 C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B), C14(H14A,H14B), C82(H82A,
 H82B), C100(H10A,H10B), C13(H13A,H13B), C80(H80A,H80B), C83(H83A,H83B),
 C81(H81A,H81B), C29(H29A,H29B), C49(H49A,H49B), C12(H12A,H12B), C32(H32A,H32B),
  C15(H15A,H15B), C46(H46A,H46B), C63(H63A,H63B), C47(H47A,H47B), C65(H65A,
 H65B), C48(H48A,H48B), C31(H31A,H31B), C30(H30A,H30B), C64(H64A,H64B),
 C66(H66A,H66B)
3.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C24(H24), C58(H58), C68(H68), C20(H20), C76(H76), C102(H102),
 C75(H75), C37(H37), C17(H17), C71(H71), C56(H56), C39(H39), C88(H88), C34(H34),
  C59(H59), C22(H22), C25(H25), C5(H5), C92(H92), C42(H42), C73(H73), C7(H7),
 C41(H41), C90(H90), C85(H85), C54(H54), C93(H93), C51(H51), C3(H3)
3.d Idealised Me refined as rotating group:
 C108(H10F,H10G,H10H), C104(H10C,H10D,H10E), C106(H10I,H10J,H10K)
3.e Idealised tetrahedral OH refined as rotating group:
 O103(H103), O107(H107), O105(H105)
;
_shelx_res_checksum              82427
_shelx_hkl_checksum              10765
_olex2_date_sample_data_collection 2022-01-18
_olex2_submission_original_sample_id 'AMS2A3A MeOH 150 K'
_olex2_submission_special_instructions 'No special instructions were received'