Conformational cooperativity between helical domains of differing geometry in oligoamide-oligourea foldamer chimeras
Julien Maury; Bryden A. F. Le Bailly; James Raftery; Jonathan Clayden; Chem.Commun. 51 (2015) 11802–; doi:10.1039/C5cc02995C

data_7117465
_publ_section_title
;
 Conformational cooperativity between helical domains of differing
 geometry in oligoamide-oligourea foldamer chimeras
;
_journal_name_full               Chem.Commun.
_journal_page_first              11802
_journal_paper_doi               10.1039/C5cc02995C
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration syn
_chemical_formula_sum            'C48 H88 N12 O12'
_chemical_formula_weight         1025.30
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-04-02 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4643(4)
_cell_length_b                   19.6586(10)
_cell_length_c                   31.9809(13)
_cell_measurement_reflns_used    7056
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.32
_cell_measurement_theta_min      4.50
_cell_volume                     5950.2(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            41565
_diffrn_reflns_theta_full        72.49
_diffrn_reflns_theta_max         72.49
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.9540
_exptl_absorpt_correction_T_min  0.838928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2224
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH, DCM, DMF'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         11298
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.088
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1275P)^2^+1.5902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1841
_refine_ls_wR_factor_ref         0.1892
_reflns_number_gt                10233
_reflns_number_total             11298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc02995c2.cif
_cod_data_source_block           s4214qa
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               7117465