Pathway complexity in fibre assembly: from liquid crystals to hyper-helical gelmorphs.
Contreras-Montoya, Rafael; Smith, James P.; Boothroyd, Stephen C.; Aguilar, Juan A.; Mirzamani, Marzieh; Screen, Martin A.; Yufit, Dmitry S.; Robertson, Mark; He, Lilin; Qian, Shuo; Kumari, Harshita; Steed, Jonathan W.; Chemical science 14 (2023) 11389–11401; doi:10.1039/d3sc03841f

data_1569985
_publ_section_title
;
 Pathway complexity in fibre assembly: from liquid crystals to
 hyper-helical gelmorphs.
;
_journal_issue                   41
_journal_name_full               'Chemical science'
_journal_page_first              11389
_journal_page_last               11401
_journal_paper_doi               10.1039/d3sc03841f
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C21 H26 N6 O4, 2(C2 H3 N)'
_chemical_formula_sum            'C25 H32 N8 O4'
_chemical_formula_weight         508.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-21
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-28 deposited with the CCDC.	2023-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.867(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.482(4)
_cell_length_b                   9.1899(15)
_cell_length_c                   17.264(3)
_cell_measurement_reflns_used    1246
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      19.88
_cell_measurement_theta_min      2.26
_cell_volume                     2774.7(9)
_computing_cell_refinement       'APEX3 v2017.3-0 (Bruker AXS, 2005-2017)'
_computing_data_collection
'Diamond I19 EH1 GDA (Allan et al., 2017), DIALS (Winter et al., 2018)'
_computing_data_reduction
'cbf_to_sfrm.py (Johnson & Probert, 2016), SAINT V8.38A (Bruker AXS, 2017)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XM  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_area_resol_mean 54.8
_diffrn_detector_type            'Dectris Pilatus 2M'
_diffrn_measured_fraction_theta_full 0.760
_diffrn_measured_fraction_theta_max 0.760
_diffrn_measurement_device
'dual air-bearing fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       '\f rotation with 0.1 degree frames'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'double crystal Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1357
_diffrn_reflns_av_unetI/netI     0.1765
_diffrn_reflns_Laue_measured_fraction_full 0.760
_diffrn_reflns_Laue_measured_fraction_max 0.760
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12165
_diffrn_reflns_point_group_measured_fraction_full 0.760
_diffrn_reflns_point_group_measured_fraction_max 0.760
_diffrn_reflns_theta_full        23.992
_diffrn_reflns_theta_max         23.992
_diffrn_reflns_theta_min         2.257
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.3726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1210 before and 0.0738 after correction.
The Ratio of minimum to maximum transmission is 0.5000.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       needle
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.004
_exptl_crystal_size_min          0.002
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.020(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.285
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         3634
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.341
_refine_ls_R_factor_all          0.2126
_refine_ls_R_factor_gt           0.1509
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3806
_refine_ls_wR_factor_ref         0.4319
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1898
_reflns_number_total             3634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03841f2.cif
_cod_data_source_block           1RR_AcNB_mix
_cod_depositor_comments
'Adding full bibliography for 1569983--1569987.cif.'
_cod_original_cell_volume        2774.6(9)
_cod_database_code               1569985
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   1.000
_shelx_estimated_absorpt_t_min   0.990
_computing_bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N3) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N4) \\sim
Ueq, Uanis(N5) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.003 and sigma for terminal
atoms of 0.006
3.a Riding coordinates:
 N1(H1), N2(H2), N3(H3), N5(H5), N6(H6)
3.b Ternary CH refined with riding coordinates:
 C6(H6A), C14(H14)
3.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
3.d Aromatic/amide H refined with riding coordinates:
 N4(H4), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21)
3.e Fitted hexagon refined as free rotating group:
 C8(C9,C10,C11,C12,C13), C16(C17,C18,C19,C20,C21)
3.f Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,H4SC)
;
_olex2_submission_special_instructions 'No special instructions were received'