Cooperative 5- and 10-membered ring interactions in the 10-helix folding of oxetin homo-oligomers.
Ragab, Sherif S.; Kassir, Ahmad F.; Guillot, Régis; Scherrmann, Marie-Christine; Boddaert, Thomas; Aitken, David J.; Chemical communications (Cambridge, England) 54 (2018) 1968–1971; doi:10.1039/c7cc09964a

data_7121213
_publ_section_title
;
 Cooperative 5- and 10-membered ring interactions in the 10-helix folding
 of oxetin homo-oligomers.
;
_journal_issue                   16
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1968
_journal_page_last               1971
_journal_paper_doi               10.1039/c7cc09964a
_journal_volume                  54
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C36 H46 N6 O15), 3(C H Cl3), 1.5(O)'
_chemical_formula_sum            'C75 H95 Cl9 N12 O32.5'
_chemical_formula_weight         2003.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-12-01 deposited with the CCDC.
2018-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.186(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.7293(9)
_cell_length_b                   20.0802(14)
_cell_length_c                   16.8259(11)
_cell_measurement_reflns_used    9019
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      66.88
_cell_measurement_theta_min      2.68
_cell_volume                     4550.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker VENTURE PHOTON100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51276
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.185
_diffrn_reflns_theta_min         2.677
_exptl_absorpt_coefficient_mu    3.293
_exptl_absorpt_correction_T_max  0.9217
_exptl_absorpt_correction_T_min  0.6891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       plate
_exptl_crystal_F_000             2084
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Flack x determined using 5921 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.021(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1168
_refine_ls_number_reflns         15990
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0864
_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^)+(0.1024P)^2^+21.1553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2252
_refine_ls_wR_factor_ref         0.2316
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                14428
_reflns_number_total             15990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09964a2.cif
_cod_data_source_block           hexamer_3
_cod_depositor_comments          'Adding full bibliography for 7121213.cif.'
_cod_original_formula_sum        'C75 H95 Cl9 N12 O32.50'
_cod_database_code               7121213
_shelx_estimated_absorpt_t_min   0.684
_shelx_estimated_absorpt_t_max   0.939
_shelx_res_checksum              1494