Synthesis and Multibromination of Nanosized Helical Aromatic Amide Foldamers via Segment-Doubling Condensation.
Li, Xuesong; Qi, Ting; Srinivas, Kolupula; Massip, Stéphane; Maurizot, Victor; Huc, Ivan; Organic letters 18 (2016) 1044–; doi:10.1021/acs.orglett.6b00165

data_1542716
_publ_section_title
;
 Synthesis and Multibromination of Nanosized Helical Aromatic Amide
 Foldamers via Segment-Doubling Condensation.
;
_journal_issue                   5
_journal_name_full               'Organic letters'
_journal_page_first              1044
_journal_paper_doi               10.1021/acs.orglett.6b00165
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C114 H105 Br7 Cl9 N16 O19'
_chemical_formula_weight         2881.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.09(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.423(4)
_cell_length_b                   23.548(5)
_cell_length_c                   30.226(6)
_cell_measurement_reflns_used    2.97
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      11140
_cell_measurement_theta_min      68.66
_cell_volume                     13687(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 (Rigaku, 2013)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 (Rigaku, 2013)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'AFC11 (Right): Eulerian 3 circle'
_diffrn_measurement_device_type  'Rigaku PILATUS conversion'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_sigmaI/netI    0.0815
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            77653
_diffrn_reflns_theta_full        68.66
_diffrn_reflns_theta_max         68.66
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    4.607
_exptl_absorpt_correction_T_max  0.7092
_exptl_absorpt_correction_T_min  0.6076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.1 (Rigaku, 2013)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5804
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
The unit cell contains at least 3 chloroform molecules which 
have been treated as a diffuse contribution to the overall scatering 
without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.777
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.500
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1390
_refine_ls_number_reflns         24823
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.502
_refine_ls_R_factor_all          0.1830
_refine_ls_R_factor_gt           0.1486
_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^)+(0.1000P)^2^+4.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3486
_refine_ls_wR_factor_ref         0.3609
_reflns_number_gt                11136
_reflns_number_total             24823
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b00165_si_002.cif
_cod_data_source_block           8mer
_cod_original_cell_volume        13686(5)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               1542716