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_7134910
_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_absolute_configuration rm
_chemical_formula_moiety         'C30 H16 F6 N4 O2'
_chemical_formula_sum            'C30 H16 F6 N4 O2'
_chemical_formula_weight         578.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_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                90
_cell_formula_units_Z            4
_cell_length_a                   10.7693(18)
_cell_length_b                   29.918(5)
_cell_length_c                   7.4885(12)
_cell_measurement_reflns_used    5282
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.3818
_cell_measurement_theta_min      2.3303
_cell_measurement_wavelength     0.71073
_cell_volume                     2412.8(7)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service v8.5.0.27 Release'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;<Phi   scan: start= 360.0; len= 180.0; end= 540.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 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= 50.00 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= 356.0; len= 224.0; end= 580.0 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   7.378 deg omega=   2.639 deg chi= -24.000 deg] 
		measure for 10.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start= 324.6; len=  72.0; end= 396.6 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=  11.068 deg phi= 360.000 deg chi=  68.500 deg] 
		measure for 10.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start=   6.8; len= 122.5; end= 129.3 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   7.378 deg phi=   0.000 deg chi= -44.500 deg] 
		measure for 10.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start= 324.6; len=  66.5; end= 391.1 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   8.475 deg phi=  36.000 deg chi=  68.500 deg] 
		measure for 10.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start=   6.8; len= 122.5; end= 129.3 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   7.378 deg phi= 306.000 deg chi= -44.500 deg] 
		measure for 10.0 seconds; frame angle 0.50 degrees, wavelength=0.71073>
<Omega scan: start=   6.8; len= 122.5; end= 129.3 at [Counterclockwise Eulerian 
angles: dx= 50.00 mm theta=   7.378 deg phi=  51.000 deg chi= -44.500 deg] 
		measure for 10.0 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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1112
_diffrn_reflns_av_unetI/netI     0.0873
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            31092
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_reduction_process narrow-frame
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.1
_diffrn_reflns_theta_min         2.01
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.399
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.942
_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 yellow'
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       plate
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 1313 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5325
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0471P)^2^+0.0324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3769
_reflns_number_total             5325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03649f2.cif
_cod_data_source_block           0365_020124_RBS6_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_database_code               7134910
_shelx_shelxl_version_number     2019/3
_exptl_bruker_absorpt_correction_t_ratio 0.7629
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.994
_diffrn_measurement_bruker_total_exposure_time 14960.0
_diffrn_reflns_bruker_av_norm_i  207.907
_diffrn_reflns_bruker_number_gt  24930
_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              19080