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_4508193
_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_moiety
'C72 H106 N12 O10, 2(C2 F3 O2), C3 H7 N O, 8(H2 O)'
_chemical_formula_sum            'C79 H129 F6 N13 O23'
_chemical_formula_weight         1742.96
_chemical_name_common            JMO-02
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-10-29T14:15:11-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.473(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.602(3)
_cell_length_b                   34.227(8)
_cell_length_c                   11.908(3)
_cell_measurement_reflns_used    5689
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.097
_cell_measurement_theta_min      0.999
_cell_measurement_wavelength     1.5418
_cell_volume                     4535(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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_detector_area_resol_mean 14
_diffrn_measured_fraction_theta_full 0
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
'1.50 degrees, 37.5 sec, detector distance 40.00 mm'
_diffrn_measurement_device       '135mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  FR591-KappaCCD2000
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0098417
_diffrn_orient_matrix_UB_12      0.0290054
_diffrn_orient_matrix_UB_13      -0.0014337
_diffrn_orient_matrix_UB_21      -0.0369944
_diffrn_orient_matrix_UB_22      0.0000000
_diffrn_orient_matrix_UB_23      -0.0867562
_diffrn_orient_matrix_UB_31      -0.0813216
_diffrn_orient_matrix_UB_32      0.0035103
_diffrn_orient_matrix_UB_33      0.0118469
_diffrn_radiation_monochromator  'graded mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5811
_diffrn_reflns_theta_full        1
_diffrn_reflns_theta_max         55.01
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1148
_refine_ls_number_reflns         5811
_refine_ls_number_restraints     1343
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1038P)^2^+1.2644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1401
_reflns_number_gt                5260
_reflns_number_total             5811
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg4007108_si_001.cif
_cod_data_source_block           Comp4
_cod_original_cell_volume        4534(2)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4508193