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_4508196
_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     'C72 H101 F5 N12 O10'
_chemical_formula_moiety         'C72 H101 F5 N12 O10, 7(O)'
_chemical_formula_sum            'C72 H101 F5 N12 O17'
_chemical_formula_weight         1501.65
_chemical_name_common            JMO-17
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_Hall           'P 61'
_space_group_name_H-M_alt        'P 61'
_symmetry_Int_Tables_number      169
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     isomor
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-11T18:40:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   48.481(15)
_cell_length_b                   48.481(15)
_cell_length_c                   10.298(2)
_cell_measurement_reflns_used    234
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.72
_cell_measurement_theta_min      1.19
_cell_measurement_wavelength     1.00614
_cell_volume                     20962(10)
_computing_cell_refinement       'MOSFLM (Leslie, 2005)'
_computing_data_collection       'DNA (Leslie, 2002)'
_computing_data_reduction        'POINTLESS and SCALA (Evans, 2006)'
_computing_molecular_graphics    'ShelXle (Hubschle, 2011)'
_computing_publication_material  'WinGX publ. routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'EPMR (Kissinger, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_type            'Dectris Pilatus3 6M'
_diffrn_measured_fraction_theta_full 0
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device       'oscillation camera'
_diffrn_measurement_device_type  'Bruker Microdiffractometer MD2M'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  'double mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.00614
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_unetI/netI     0.0716
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            53474
_diffrn_reflns_theta_full        1
_diffrn_reflns_theta_max         23.72
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALA (Evans, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4788
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.32
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.0066(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.606
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         3837
_refine_ls_number_restraints     1358
_refine_ls_restrained_S_all      1.405
_refine_ls_R_factor_all          0.1417
_refine_ls_R_factor_gt           0.1357
_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          0.31
_refine_ls_wR_factor_ref         0.3179
_reflns_number_gt                3307
_reflns_number_total             3837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg4007108_si_004.cif
_cod_data_source_block           Comp14
_cod_original_cell_volume        20962(16)
_cod_database_code               4508196