Postsynthetic Modification of C~3~-Symmetric Aza-β^3^-Cyclohexapeptides
Philippe Le Grel; Arnaud Salaün; Clémence Mocquet; Barbara Le Grel; Thierry Roisnel; Michel Potel; Journal of Organic Chemistry 73 (2008) 1306–1310; doi:10.1021/jo7021394

data_4023258
_publ_section_title
;
 Postsynthetic Modification of C~3~-Symmetric
 Aza-\b^3^-Cyclohexapeptides
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1306
_journal_page_last               1310
_journal_paper_doi               10.1021/jo7021394
_journal_volume                  73
_journal_year                    2008
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H63 N15 O9'
_chemical_formula_sum            'C36 H63 N15 O9'
_chemical_formula_weight         850.01
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      146
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2007-09-12T16:12:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.5180(10)
_cell_length_b                   18.5180(10)
_cell_length_c                   13.4400(10)
_cell_measurement_reflns_used    7503
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      1.98
_cell_measurement_wavelength     0.71073
_cell_volume                     3991.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by SAINT Bruker-AXS'
_diffrn_orient_matrix_UB_11      0.199252E-1
_diffrn_orient_matrix_UB_12      -0.83103E-2
_diffrn_orient_matrix_UB_13      -0.658535E-1
_diffrn_orient_matrix_UB_21      -0.420726E-1
_diffrn_orient_matrix_UB_22      0.99898E-2
_diffrn_orient_matrix_UB_23      -0.344686E-1
_diffrn_orient_matrix_UB_31      0.414838E-1
_diffrn_orient_matrix_UB_32      0.60985E-1
_diffrn_orient_matrix_UB_33      -0.33275E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23506
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.96
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.3
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2026
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0987P)^2^+0.6763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1322
_reflns_number_gt                1933
_reflns_number_total             2026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo7021394_si2.cif
_cod_data_source_block           c3isoallyl
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4023258