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_4508194
_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, C2 F3 O2, 20 O'
_chemical_formula_sum            'C74 H106 F3 N12 O32'
_chemical_formula_weight         1732.71
_chemical_name_common            JMO-04
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           169
_symmetry_cell_setting           hexagonal
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-06-27T11:42:18-00:00
_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                   27.931(1)
_cell_length_b                   27.931(1)
_cell_length_c                   22.523(2)
_cell_measurement_reflns_used    5855
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      51.874
_cell_measurement_theta_min      0.982
_cell_measurement_wavelength     1.5418
_cell_volume                     15217.0(16)
_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 1
_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      0.0266598
_diffrn_orient_matrix_UB_12      0.0351577
_diffrn_orient_matrix_UB_13      0.0204649
_diffrn_orient_matrix_UB_21      -0.0240397
_diffrn_orient_matrix_UB_22      -0.0120199
_diffrn_orient_matrix_UB_23      0.0361216
_diffrn_orient_matrix_UB_31      0.0205052
_diffrn_orient_matrix_UB_32      -0.0181267
_diffrn_orient_matrix_UB_33      0.0157405
_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_unetI/netI     0.017
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5837
_diffrn_reflns_theta_full        1
_diffrn_reflns_theta_max         51.84
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5502
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.37
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.0014(3)
_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   1.822
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1408
_refine_ls_number_reflns         5837
_refine_ls_number_restraints     2059
_refine_ls_restrained_S_all      1.636
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_gt           0.1302
_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          0.3355
_refine_ls_wR_factor_ref         0.3451
_reflns_number_gt                5280
_reflns_number_total             5837
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg4007108_si_002.cif
_cod_data_source_block           Comp6
_cod_original_cell_volume        15217(2)
_cod_database_code               4508194