Coaxial assembly of helical aromatic foldamers by metal coordination.
Galan, Albano; Lulic, Kristijan; Wang, Jingqi; Wicher, Barbara; Huc, Ivan; Duhamel, Jean; Maurizot, Victor; Chemical communications (Cambridge, England) 59 (2023) 5253–5256; doi:10.1039/d3cc00866e

data_7131516
_publ_section_title
;
 Coaxial assembly of helical aromatic foldamers by metal coordination.
;
_journal_issue                   35
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5253
_journal_page_last               5256
_journal_paper_doi               10.1039/d3cc00866e
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C224 H226 K2 N32 O40, [+ solvents]'
_chemical_formula_sum            'C224 H226 K2 N32 O40'
_chemical_formula_weight         4084.55
_chemical_properties_physical    Air-sensitive
_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   geom
_audit_creation_date             2023-03-24
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-03-27 deposited with the CCDC.	2023-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                66.462(12)
_cell_angle_beta                 88.27(2)
_cell_angle_gamma                80.27(2)
_cell_formula_units_Z            2
_cell_length_a                   19.053(4)
_cell_length_b                   24.368(4)
_cell_length_c                   26.337(5)
_cell_measurement_reflns_used    3226
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      60.3
_cell_measurement_theta_min      18.9
_cell_volume                     11040(4)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b43, Rigaku 2015'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b43, Rigaku 2015'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b43, Rigaku 2015'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 13.333
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0862
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            117829
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        58.936
_diffrn_reflns_theta_max         58.936
_diffrn_reflns_theta_min         1.831
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_current           66.0
_diffrn_source_power             2.97
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 2.1 b43 (Rigaku, 2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4304
_exptl_crystal_recrystallization_method
'n-hexane to a chloroform solution of the dimer through a dichloromethane buffer solution'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2549
_refine_ls_number_reflns         31068
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1804
_refine_ls_R_factor_gt           0.0989
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2756
_refine_ls_wR_factor_ref         0.3316
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13719
_reflns_number_total             31068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00866e2.cif
_cod_data_source_block           q8-k-q8
_cod_depositor_comments
'Adding full bibliography for 7131515--7131517.cif.'
_cod_database_code               7131516
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.748
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C17B-C18B = C18B-C19B = C18B-C20B
 1.51 with sigma of 0.001
 C19B-C20B
 2.5 with sigma of 0.001
 C20D-C18D
 1.51 with sigma of 0.002
 C19D-C18D
 1.51 with sigma of 0.002
 C2D-C1D
 1.51 with sigma of 0.002
 C9B-C10B
 1.51 with sigma of 0.002
 C80A-C78A
 1.51 with sigma of 0.002
 C80C-C78C
 1.51 with sigma of 0.002
 C17B-C47A
 2.9 with sigma of 0.02
3. Rigid bond restraints
 C10B, C12B, C11B, C9B, O3B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C53C, C54C, C55C, C56C, C57C, C58C, N12C, C59C, C51C, C52C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uiso(C17B) = Uiso(C19B) = Uiso(C18B) = Uiso(C20B)
Uiso(C17D) = Uiso(C18D) = Uiso(C20D) = Uiso(C19D)
Uanis(C14B) = Uanis(C16B) = Uanis(C15B) = Uanis(C13B)
5.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C4A(H4A), C7A(H7A), C12A(H12A), C13A(H13A), C14A(H14A),
 C17A(H17A), C22A(H22A), C23A(H23A), C24A(H24A), C27A(H27A), C32A(H32A),
 C33A(H33A), C34A(H34A), C37A(H37A), C42A(H42A), C43A(H43A), C44A(H44A),
 C47A(H47A), C52A(H52A), C53A(H53A), C54A(H54A), C57A(H57A), C62A(H62A),
 C63A(H63A), C64A(H64A), C67A(H67A), C72A(H72A), C73A(H73A), C74A(H74A),
 C77A(H77A), N3A(H3AA), N5A(H5A), N7A(H7AA), N9A(H9A), N11A(H11A), N13A(H13B),
 N15A(H15A), C2C(H2C), C3C(H3C), C4C(H4C), C7C(H7C), C12C(H12C), C13C(H13C),
 C14C(H14C), C17C(H17C), C22C(H22C), C23C(H23C), C24C(H24C), C27C(H27C),
 C32C(H32C), C33C(H33C), C34C(H34C), C37C(H37C), C42C(H42C), C43C(H43C),
 C44C(H44C), C47C(H47C), C52C(H52C), C53C(H53C), C54C(H54C), C57C(H57C),
 C62C(H62C), C63C(H63C), C64C(H64C), C67C(H67C), C72C(H72C), C73C(H73C),
 C74C(H74C), C77C(H77C), N3C(H3CA), N5C(H5C), N7C(H7CA), N9C(H9C), N11C(H11C),
 N13C(H13D), N15C(H15C)
;
_shelx_res_checksum              31378
_shelx_hkl_checksum              80591
_shelx_fab_checksum              97179
_olex2_submission_special_instructions 'No special instructions were received'