Halogen and hydrogen bonding-driven self-assembly of supramolecular macrocycles and double helices from hydrogen-bonded arylamide foldamers
Koppireddi, Satish; Liu, Chuan-Zhi; Wang, Hui; Zhang, Dan-Wei; Li, Zhan-Ting; CrystEngComm 21 (2019) 2626–; doi:10.1039/C8CE02187B

data_7232473
_publ_section_title
;
 Halogen and hydrogen bonding-driven self-assembly of supramolecular
 macrocycles and double helices from hydrogen-bonded arylamide foldamers
;
_journal_issue                   16
_journal_name_full               CrystEngComm
_journal_page_first              2626
_journal_paper_doi               10.1039/C8CE02187B
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         '1.5(C6 F4 I2), C34 H46 N4 O6'
_chemical_formula_sum            'C43 H46 F6 I3 N4 O6'
_chemical_formula_weight         1209.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-12-26 deposited with the CCDC.    2019-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                116.2490(10)
_cell_angle_beta                 96.2380(10)
_cell_angle_gamma                100.8410(10)
_cell_formula_units_Z            2
_cell_length_a                   9.3189(3)
_cell_length_b                   16.8147(5)
_cell_length_c                   18.3190(6)
_cell_measurement_reflns_used    9078
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.13
_cell_measurement_theta_min      2.28
_cell_volume                     2467.84(14)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28784
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.374
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.969
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6876
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0602 before and 0.0425 after correction. The Ratio of minimum to maximum transmission is 0.9221. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1186
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         8618
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+2.2823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6635
_reflns_number_total             8618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce02187b2.cif
_cod_data_source_block           z
_cod_depositor_comments
'Adding full bibliography for 7232470--7232474.cif.'
_cod_database_code               7232473
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.770
_shelx_estimated_absorpt_t_min   0.546
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C26 \\sim C27: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
3.a Ternary CH refined with riding coordinates:
 C18(H18), C22(H22), C26(H26), C30(H30)
3.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C21(H21A,H21B), C25(H25A,H25B), C29(H29A,H29B)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12),
 C15(H15)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C)
;
_shelx_res_checksum              80394
_shelx_fab_checksum              64366
_olex2_submission_special_instructions 'No special instructions were received'