Anion-Binding Properties of a Cyclic Pseudohexapeptide Containing 1,5-Disubstituted 1,2,3-Triazole Subunits
Martin R. Krause; Richard Goddard; Stefan Kubik; Journal of Organic Chemistry 76 (2011) 7084–7095; doi:10.1021/jo201024r

data_4026558
_publ_section_title
;
 Anion-Binding Properties of a Cyclic Pseudohexapeptide Containing
 1,5-Disubstituted 1,2,3-Triazole Subunits
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7084
_journal_page_last               7095
_journal_paper_doi               10.1021/jo201024r
_journal_volume                  76
_journal_year                    2011
_chemical_absolute_configuration rm
_chemical_compound_source        acetone,hexane
_chemical_formula_moiety         'C30 H27 N15 O3, C3 H6 O, H2 O'
_chemical_formula_sum            'C33 H35 N15 O5'
_chemical_formula_weight         721.76
_chemical_name_systematic
;
cyclo-tris-((R)ethyl-1,5-triazol-2,6-pyridyl-amino-carbonyl)
acetone hydrate solute
;
_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_block_code                MK-485
_audit_creation_date             2011-05-05
_cell_angle_alpha                90.00
_cell_angle_beta                 101.469(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9601(9)
_cell_length_b                   9.3717(9)
_cell_length_c                   19.2123(18)
_cell_measurement_reflns_used    9639
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.6524
_cell_measurement_theta_min      3.0125
_cell_volume                     1757.5(3)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (G. M. Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (G. M. Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            103103
_diffrn_reflns_theta_full        32.89
_diffrn_reflns_theta_max         32.89
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.99674
_exptl_absorpt_correction_T_min  0.99112
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       prism
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.820
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         6846
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.820
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0937P)^2^+0.3454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                6524
_reflns_number_total             6846
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo201024r_si_005.cif
_cod_data_source_block           10.acetone.water
_cod_original_sg_symbol_Hall     'p 2yb'
_cod_database_code               4026558