Ring-chain equilibria of dynamic macrocycles with a bis(hindered amino)disulfide linker
Takashima, Rikito; Aoki, Daisuke; Kuwata, Shigeki; Otsuka, Hideyuki; Polymer Chemistry 14 (2023) 4344–4351; doi:10.1039/D3PY00808H

data_1569802
_publ_section_title
;
 Ring-chain equilibria of dynamic macrocycles with a bis(hindered
 amino)disulfide linker
;
_journal_issue                   37
_journal_name_full               'Polymer Chemistry'
_journal_page_first              4344
_journal_page_last               4351
_journal_paper_doi               10.1039/D3PY00808H
_journal_volume                  14
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C29 H52 N2 O4 S4'
_chemical_formula_sum            'C29 H52 N2 O4 S4'
_chemical_formula_weight         620.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2023-05-08 deposited with the CCDC.	2023-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.944(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            36
_cell_length_a                   28.460(2)
_cell_length_b                   45.626(3)
_cell_length_c                   23.4507(17)
_cell_measurement_reflns_used    30745
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     30434(4)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b46'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b46 (Rigaku, 2016)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b46'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1566
_diffrn_reflns_av_unetI/netI     0.1392
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       59
_diffrn_reflns_limit_k_min       -59
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            166950
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         3.030
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.315
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             12096.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethyl acetate/heptane'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.05
_refine_diff_density_min         -0.95
_refine_ls_abs_structure_details
;
 No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.45(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     3249
_refine_ls_number_reflns         68028
_refine_ls_number_restraints     91
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0915
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1287P)^2^+39.0130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2342
_refine_ls_wR_factor_ref         0.2555
_reflns_Friedel_coverage         0.956
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                54418
_reflns_number_total             68028
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d3py00808h2.cif
_cod_data_source_block           MMC5S
_cod_depositor_comments
'Adding full bibliography for 1569801--1569802.cif.'
_cod_database_code               1569802
_shelx_res_checksum              24013