Foldamer engineering with squaramide and phenanthroline motifs: synthesis, characterisation, and structural insights.
Benny, Renitta; Andrews, Alex P.; De, Soumen; Chemical communications (Cambridge, England) 61 (2025) 14955–14958; doi:10.1039/d5cc03649f

data_7134911
_publ_section_title
;
 Foldamer engineering with squaramide and phenanthroline motifs:
 synthesis, characterisation, and structural insights.
;
_journal_issue                   77
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14955
_journal_page_last               14958
_journal_paper_doi               10.1039/d5cc03649f
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C68 H40 N10 O4, 2(C3 H7 N O)'
_chemical_formula_sum            'C74 H54 N12 O6'
_chemical_formula_weight         1207.29
_space_group_crystal_system      trigonal
_space_group_IT_number           145
_space_group_name_Hall           'P 32'
_space_group_name_H-M_alt        'P 32'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;FinalCif 2024.9-0 by Daniel Kratzert, Freiburg 2025, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-06-27 deposited with the CCDC.	2025-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   17.1456(3)
_cell_length_b                   17.1456(3)
_cell_length_c                   16.9139(5)
_cell_measurement_reflns_used    9795
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.1175
_cell_measurement_theta_min      2.6637
_cell_measurement_wavelength     0.71073
_cell_volume                     4306.06(17)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1503)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.391
_diffrn_detector_type            'Bruker PHOTON III C14'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;<Phi   scan: start= 360.0; len= 180.0; end= 540.0 at [Counterclockwise Eulerian 
angles: dx= 45.00 mm theta=   0.000 deg omega=   0.000 deg chi=  54.740 deg] 
		measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Phi   scan: start= 180.0; len= 180.0; end= 360.0 at [Counterclockwise Eulerian 
angles: dx= 45.00 mm theta=   0.000 deg omega=   0.000 deg chi=  54.740 deg] 
		measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=0.71073>
<Phi   scan: start= 158.9; len= 154.0; end= 312.9 at [Counterclockwise Eulerian 
angles: dx= 45.00 mm theta=   5.815 deg omega=   5.450 deg chi= -24.000 deg] 
		measure for 7.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start=   7.0; len= 114.5; end= 121.5 at [Counterclockwise Eulerian 
angles: dx= 45.00 mm theta=   5.815 deg phi=   0.000 deg chi= -44.500 deg] 
		measure for 7.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Phi   scan: start= 158.9; len= 146.0; end= 304.9 at [Counterclockwise Eulerian 
angles: dx= 45.00 mm theta=   5.815 deg omega=   6.048 deg chi= -44.500 deg] 
		measure for 7.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start=   7.0; len= 114.5; end= 121.5 at [Counterclockwise Eulerian 
angles: dx= 45.00 mm theta=   5.815 deg phi=  72.000 deg chi= -44.500 deg] 
		measure for 7.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
;
_diffrn_measurement_device       'Bruker D8 QUEST'
_diffrn_measurement_device_type  'Four-circle Kappa diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support Fibre-loope
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_probe          'Mo K\a'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            82588
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_reduction_process narrow-frame
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.295
_diffrn_reflns_theta_min         2.376
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.404
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for single-crystal
 structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            'clear intense red'
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_meas      1.397
_exptl_crystal_density_method    NONE
_exptl_crystal_description       block
_exptl_crystal_F_000             1890
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 5926 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         14244
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0724P)^2^+0.7913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1206
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                13095
_reflns_number_total             14244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03649f2.cif
_cod_data_source_block           RB3P3S_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7134910--7134912.cif.
;
_cod_original_cell_volume        4306.1(2)
_cod_database_code               7134911
_shelx_shelxl_version_number     2019/3
_exptl_bruker_absorpt_correction_t_ratio 0.917
_shelx_estimated_absorpt_t_min   0.981
_shelx_estimated_absorpt_t_max   0.988
_diffrn_measurement_bruker_total_exposure_time 7766.0
_diffrn_reflns_bruker_av_norm_i  1132.766
_diffrn_reflns_bruker_number_gt  82901
_computing_bruker_data_scaling
'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction'
_geom_details
; All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
_shelx_res_checksum              79683