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_1569987
_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_absolute_configuration unk
_chemical_formula_moiety         'C21 H26 N6 O4, 2(H2 O)'
_chemical_formula_sum            'C21 H30 N6 O6'
_chemical_formula_weight         462.51
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2019-05-15
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-11-28 deposited with the CCDC.	2023-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.897(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.300(3)
_cell_length_b                   4.5408(11)
_cell_length_c                   21.909(5)
_cell_measurement_reflns_used    2808
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.15
_cell_measurement_theta_min      2.49
_cell_volume                     1124.0(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS, 2016)'
_computing_data_collection       'GDA 8.44; generic data acquisition software'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'Dectris Pilatus 2M'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       '\f and \w rotation with 0.1 degree frames'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.2213
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11700
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_min         0.901
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1353 before and 0.0469 after correction. 
The Ratio of minimum to maximum transmission is 0.4009. 
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    1.366
_exptl_crystal_description       needle
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.012
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.5207
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 488 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -1.8(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5176
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1761
_refine_ls_R_factor_gt           0.1179
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1410P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3080
_refine_ls_wR_factor_ref         0.3656
_reflns_Friedel_coverage         0.777
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                2685
_reflns_number_total             5176
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03841f2.cif
_cod_data_source_block           1RR_DH_19srv179
_cod_depositor_comments
'Adding full bibliography for 1569983--1569987.cif.'
_cod_original_cell_volume        1124.1(5)
_cod_database_code               1569987
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   1.000
_shelx_estimated_absorpt_t_min   0.983
_computing_bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.969(2)
 0.031(2)
2. 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, All O(H,H) groups
3.a Free rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
3.b Ternary CH refined with riding coordinates:
 C1(H1A), C7(H7)
3.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
3.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21)
3.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_olex2_submission_special_instructions 'No special instructions were received'