Small Head-to-Tail Macrocyclic α-Peptoids.
Culf, Adrian S.; Cuperlović-Culf, Miroslava; Léger, Daniel A; Decken, Andreas; Organic letters 16 (2014) 2780–2783; doi:10.1021/ol501102b

data_1515991
_publ_section_title
;
 Small Head-to-Tail Macrocyclic \a-Peptoids.
;
_journal_issue                   10
_journal_name_full               'Organic letters'
_journal_page_first              2780
_journal_page_last               2783
_journal_paper_doi               10.1021/ol501102b
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C45 H45 N5 O5, 0.5 [C H Cl3]'
_chemical_formula_sum            'C45.5 H45.5 Cl1.5 N5 O5'
_chemical_formula_weight         795.54
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 102.463(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.448(16)
_cell_length_b                   13.284(6)
_cell_length_c                   27.047(12)
_cell_measurement_reflns_used    5041
_cell_measurement_temperature    188(1)
_cell_measurement_theta_max      22.23
_cell_measurement_theta_min      2.46
_cell_volume                     8577(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      188(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker AXS SMART1000/P4'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_av_sigmaI/netI    0.1463
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            27610
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.54
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              K760
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  0.9831
_exptl_absorpt_correction_T_min  0.9046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rod
_exptl_crystal_F_000             3352
_exptl_crystal_recrystallization_method 'CHCl3, EtOH'
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         9556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.2204
_refine_ls_R_factor_gt           0.1180
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1878P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3592
_refine_ls_wR_factor_ref         0.3831
_reflns_number_gt                3630
_reflns_number_total             9556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol501102b_si_005.cif
_cod_data_source_block           ac131170
_cod_depositor_comments
'Adding full bibliography for 1515988--1515991.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C45.50 H45.50 Cl1.50 N5 O5'
_cod_database_code               1515991