Design, Synthesis, and Structural Analysis of Turn Modifiedcyclo-(αβ3αβ2α)2Peptide Derivatives toward Crystalline Hexagon-Shaped Cationic Nanochannel Assemblies
Otero, José M.; van der Knaap, Matthijs; Llamas-Saiz, Antonio L.; van Raaij, Mark J.; Amorín, Manuel; Granja, Juan R.; Filippov, Dmitri V.; van der Marel, Gijsbert A.; Overkleeft, Herman S.; Overhand, Mark; Crystal Growth & Design 13 (2013) 4355–; doi:10.1021/cg4007108

data_4508198
_publ_section_title
;
 Design, Synthesis, and Structural Analysis of Turn
 Modifiedcyclo-(\a\b3\a\b2\a)2Peptide Derivatives toward Crystalline
 Hexagon-Shaped Cationic Nanochannel Assemblies
;
_journal_issue                   10
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4355
_journal_paper_doi               10.1021/cg4007108
_journal_volume                  13
_journal_year                    2013
_chemical_absolute_configuration syn
_chemical_compound_source        'synthesis as described'
_chemical_formula_analytical     'C60 H94 N12 O10'
_chemical_formula_moiety         '1.5(C60 H94 N12 O10), 1(C2 F3 O2), 14(O)'
_chemical_formula_sum            'C92 H141 F3 N18 O31'
_chemical_formula_weight         2052.23
_chemical_name_common            DM74
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-09-28T10:48:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.635(5)
_cell_length_b                   38.582(10)
_cell_length_c                   28.317(3)
_cell_measurement_temperature    100(2)
_cell_volume                     24729(9)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'DNA (Leslie, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'CCD Q315r ADSC X'
_diffrn_measurement_method       'oscillation camera'
_diffrn_radiation_monochromator  'double mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.9537
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36301
_diffrn_reflns_theta_full        1
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_min         1.4
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             8752
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.67
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1555
_refine_ls_number_reflns         6760
_refine_ls_number_restraints     2123
_refine_ls_restrained_S_all      2.004
_refine_ls_R_factor_all          0.1583
_refine_ls_R_factor_gt           0.1498
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3933
_refine_ls_wR_factor_ref         0.4063
_reflns_number_gt                6099
_reflns_number_total             6760
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg4007108_si_006.cif
_cod_data_source_block           Comp18
_cod_database_code               4508198