Self-Assembly of Noncyclic Bis-D- and L-tripeptides into Higher Order Tubular Constructs: Design, Synthesis, and X-ray Crystal Superstructure
Stephen Hanessian; Valerio Vinci; Kamal Fettis; Thierry Maris; Minh Tan Phan Viet; Journal of Organic Chemistry 73 (2008) 1181–1191; doi:10.1021/jo701621c

data_4023248
_publ_section_title
;
 Self-Assembly of Noncyclic Bis-D- and L-tripeptides into Higher Order
 Tubular Constructs: Design, Synthesis, and X-ray Crystal Superstructure
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1181
_journal_page_last               1191
_journal_paper_doi               10.1021/jo701621c
_journal_volume                  73
_journal_year                    2008
_chemical_absolute_configuration rmad
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         '2 (C76 H94 Br2 N8 O16), 2 (C6 H6), C H Cl3'
_chemical_formula_sum            'C165 H201 Br4 Cl3 N16 O32'
_chemical_formula_weight         3346.41
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.146(2)
_cell_length_b                   26.468(3)
_cell_length_c                   35.413(3)
_cell_measurement_reflns_used    456
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.00
_cell_measurement_theta_min      4.35
_cell_volume                     17008(3)
_computing_cell_refinement       'SMART (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'UdMX (local program)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir2002 (Burla, 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker AXS Smart 4K/Platform'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'MonteL 100 Multi Layer Optic'
_diffrn_radiation_source
'Rotating Anode FR591 6KW 100 micron focal spot '
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.055
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            167546
_diffrn_reflns_theta_full        68.05
_diffrn_reflns_theta_max         68.05
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        -1.20
_diffrn_standards_interval_time  1440
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    2.196
_exptl_absorpt_correction_T_max  0.9000
_exptl_absorpt_correction_T_min  0.7800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             7000
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), 12233 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.10(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1886
_refine_ls_number_reflns         28888
_refine_ls_number_restraints     618
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0888
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0830P)^2^ + 11.5670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2119
_refine_ls_wR_factor_ref         0.2133
_reflns_number_gt                17224
_reflns_number_total             28888
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo701621c-File003.cif
_cod_data_source_block           han398
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4023248