Redox-controlled hybridization of helical foldamers
Faour, Lara; Adam, Catherine; Gautier, Christelle; Goeb, Sebastien; Allain, Magali; LEVILLAIN, Eric; Canevet, David; Salle, Marc; Chemical Communications  (2019) –; doi:10.1039/C9CC02498K

data_7123306
_publ_section_title
;
 Redox-controlled hybridization of helical foldamers
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02498K
_journal_year                    2019
_chemical_formula_moiety         'C63 H61 N17 O9 S8, 5(C H4 O)'
_chemical_formula_sum            'C68 H81 N17 O14 S8'
_chemical_formula_weight         1616.97
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-05-23T10:46:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-01-18 deposited with the CCDC.    2019-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.900(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.915(3)
_cell_length_b                   29.802(5)
_cell_length_c                   15.018(2)
_cell_measurement_reflns_used    1509
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      58.427
_cell_measurement_theta_min      2.976
_cell_volume                     7570(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector_area_resol_mean 5.199
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_unetI/netI     0.0975
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16017
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        70
_diffrn_reflns_theta_max         73.695
_diffrn_reflns_theta_min         2.966
_exptl_absorpt_coefficient_mu    2.807
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.52226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       needle
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.056
_platon_squeeze_details
;
The structure refinement showed disordered electron density which could not be
 reliably modeled and the program PLATON/SQUEEZE were used to remove the
scattering contribution corresponding to methanol solvent from the intensity
 data. The unit cell contains 8 voids of total volume of 1196 A3 containing
348 electrons which can be attributed to approximately 20 methanol molecules
in the unit cell. The solvent composition was included in the calculation of
the empirical formula, formula weight, density, linear absorption coefficient
        and F(000).
;
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7172
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.2038
_refine_ls_R_factor_gt           0.1199
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1868P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3202
_refine_ls_wR_factor_ref         0.3892
_reflns_Friedel_coverage         0
_reflns_number_gt                2420
_reflns_number_total             7172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02498k2.cif
_cod_data_source_block           platon_sqd
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7123306
_platon_squeeze_void_probe_radius 1.2