Supramolecular interactions between ethylene-bridged oligoureas: nanorings and chains formed by cooperative positive allostery
Tilly, David P.; Žabka, Matej; Vitorica-Yrzebal, Inigo; Sparkes, Hazel Anne; Pridmore, Natalie E.; Clayden, Jonathan; Chemical Science  (2022) –; doi:10.1039/D2SC04716K

data_1567845
_publ_section_title
;
 Supramolecular interactions between ethylene-bridged oligoureas:
 nanorings and chains formed by cooperative positive allostery
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC04716K
_journal_year                    2022
_chemical_formula_moiety         'C H Cl3, C30 H26 F12 N6 O4'
_chemical_formula_sum            'C31 H27 Cl3 F12 N6 O4'
_chemical_formula_weight         881.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-01
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392)
;
_audit_update_record
;
2022-08-08 deposited with the CCDC.	2022-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                80.719(2)
_cell_angle_beta                 76.811(2)
_cell_angle_gamma                73.555(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9480(4)
_cell_length_b                   12.5972(5)
_cell_length_c                   12.9273(4)
_cell_measurement_reflns_used    3077
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.27
_cell_measurement_theta_min      2.19
_cell_volume                     1807.12(11)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'Bruker Apex suite'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7730
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.868
_diffrn_reflns_theta_min         1.627
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.362
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 43556 reflections, Rint = 0.0537
 (15599 with I > 3sig(I), Rint = 0.0322)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       block
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.476
_exptl_crystal_size_mid          0.385
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         7730
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0410P)^2^+1.6732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1262
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5636
_reflns_number_total             7730
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04716k2.cif
_cod_data_source_block           hklf5
_cod_database_code               1567845
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.846
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51902
 0.48098
2. Restrained distances
 Cl1A-C31 \\sim Cl1-C31 \\sim Cl3A-C31 \\sim Cl3-C31 \\sim Cl2A-C31 \\sim
Cl2-C31
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl1A \\sim Cl1 \\sim Cl3A \\sim Cl3 \\sim Cl2A \\sim Cl2: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(H31A)=Sof(Cl2A)=Sof(Cl1A)=Sof(Cl3A)=1-FVAR(1)
 Sof(Cl3)=Sof(Cl2)=Sof(Cl1)=Sof(H31)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C31(H31), C31(H31A)
5.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C10(H10A,H10B), C21(H21A,H21B), C11(H11A,H11B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1A), C17(H17), C5(H5A), C18(H18), C3(H3), C15(H15), C14(H14), C28(H28),
 C24(H24), C26(H26)
5.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_shelx_res_checksum              19308
_shelx_hkl_checksum              37048
_olex2_submission_special_instructions 'No special instructions were received'