Adaptive Covalent Networks Enabled by Dual Reactivity: The Evolution of Reversible Covalent Bonds, Their Molecular Assemblies, and Guest Recognition.
Mao, Jialin; Hai, Yu; Ye, Hebo; You, Lei; The Journal of organic chemistry 85 (2020) 5351–5361; doi:10.1021/acs.joc.0c00051

data_4038232
_publ_section_title
;
 Adaptive Covalent Networks Enabled by Dual Reactivity: The Evolution of
 Reversible Covalent Bonds, Their Molecular Assemblies, and Guest
 Recognition.
;
_journal_issue                   8
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5351
_journal_page_last               5361
_journal_paper_doi               10.1021/acs.joc.0c00051
_journal_volume                  85
_journal_year                    2020
_chemical_formula_moiety         'C28 H32 N4 O4 S2'
_chemical_formula_sum            'C28 H32 N4 O4 S2'
_chemical_formula_weight         552.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                95.055(4)
_cell_angle_beta                 95.992(4)
_cell_angle_gamma                100.265(5)
_cell_formula_units_Z            4
_cell_length_a                   8.0998(5)
_cell_length_b                   11.0792(6)
_cell_length_c                   30.7422(9)
_cell_measurement_reflns_used    12503
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      60.2130
_cell_measurement_theta_min      2.5230
_cell_volume                     2683.7(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            37170
_diffrn_reflns_theta_full        27.61
_diffrn_reflns_theta_max         27.61
_diffrn_reflns_theta_min         1.34
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1330
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         12071
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1447
_refine_ls_R_factor_gt           0.1150
_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^)+(0.0814P)^2^+17.4010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3299
_refine_ls_wR_factor_ref         0.3434
_reflns_number_gt                8145
_reflns_number_total             12071
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo0c00051_si_002.cif
_cod_data_source_block           2C
_cod_depositor_comments
'Adding full bibliography for 4038227--4038237.cif.'
_cod_database_code               4038232
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C52(H52), C8(H8), C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C23(H23A,H23B), C31(H31A,H31B), C44(H44A,H44B), C53(H53A,
 H53B), C67(H67A,H67B), C68(H68A,H68B), C71(H71A,H71B), C29(H29A,H29B),
 C30(H30A,H30B), C34(H34A,H34B), C39(H39A,H39B), C41(H41A,H41B), C45(H45A,H45B),
  C56(H56A,H56B), C62(H62A,H62B)
2.c Aromatic/amide H refined with riding coordinates:
 N22(H22), C40(H40), C48(H48), C50(H50), C51(H51), C55(H55), C57(H57),
 C58(H58), C60(H60), N61(H61), C63(H63), C64(H64), C69(H69), C70(H70), N3(H3),
 N10(H10), C25(H25), C32(H32), C33(H33), C35(H35), C37(H37), C47(H47), C49(H49),
  C54(H54), C59(H59), C65(H65), C66(H66), C72(H72)
;
_olex2_submission_special_instructions 'No special instructions were received'