The synthesis of head-to-tail cyclic sulfono-γ-AApeptides.
Wu, Haifan; She, Fengyu; Gao, Wenyang; Prince, Austin; Li, Yaqiong; Wei, Lulu; Mercer, Allison; Wojtas, Lukasz; Ma, Shengqian; Cai, Jianfeng; Organic & biomolecular chemistry 13 (2015) 672–676; doi:10.1039/c4ob02232g

data_7154201
_publ_section_title
;
 The synthesis of head-to-tail cyclic sulfono-\g-AApeptides.
;
_journal_issue                   3
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              672
_journal_page_last               676
_journal_paper_doi               10.1039/c4ob02232g
_journal_volume                  13
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety
'2(C33 H39 Cl3 N6 O9 S3), 3.15(C H Cl3), 0.5 (C2 H O2 F3)'
_chemical_formula_sum            'C70.15 H81.65 Cl15.44 F1.5 N12 O19 S6'
_chemical_formula_weight         2165.20
_chemical_name_common            hw_c_17_2
_chemical_name_systematic        5
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1143(4)
_cell_length_b                   20.8803(6)
_cell_length_c                   26.8416(6)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.08
_cell_measurement_theta_min      3.06
_cell_volume                     9591.9(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0936
_diffrn_reflns_av_unetI/netI     0.1036
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            50593
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.197
_diffrn_reflns_theta_min         3.723
_diffrn_source                   'INCOATEC Imus micro-focus source'
_exptl_absorpt_coefficient_mu    5.886
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS,BRUKER 2014'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       needle
_exptl_crystal_F_000             4442
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 4104 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.058(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1169
_refine_ls_number_reflns         17264
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+4.8246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1828
_reflns_Friedel_coverage         0.822
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.972
_reflns_number_gt                11901
_reflns_number_total             17264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ob02232g2.cif
_cod_data_source_block           hw_c_17_2_0m
_cod_depositor_comments          'Adding full bibliography for 7154201.cif.'
_cod_original_formula_sum        'C70.15 H81.65 Cl15.44 F1.50 N12 O19 S6'
_cod_database_code               7154201
_shelx_estimated_absorpt_t_min   0.619
_shelx_estimated_absorpt_t_max   0.891
_shelxl_version_number           2014-3
_shelx_res_checksum              69423