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_4038236
_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_absolute_configuration unk
_chemical_formula_moiety         'C27 H28 N2 O4 S4'
_chemical_formula_sum            'C27 H28 N2 O4 S4'
_chemical_formula_weight         572.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_Int_Tables_number      18
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-19
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.760(5)
_cell_length_b                   25.156(11)
_cell_length_c                   6.3059(13)
_cell_measurement_reflns_used    2848
_cell_measurement_temperature    301.45(10)
_cell_measurement_theta_max      57.2070
_cell_measurement_theta_min      2.6840
_cell_volume                     2658.7(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      301.45(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.8566
_diffrn_measured_fraction_theta_max 0.8566
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     62.00 129.00   0.50    0.75    --   70.46  58.00-121.00  134
  2  \w     81.00 133.00   0.50    0.75    --   70.46  88.00 -13.00  104
  3  \w     54.00 129.00   0.50    0.75    --   70.46  57.00 150.00  150
  4  \w     -1.00  59.00   0.50    0.75    --   70.46 -78.00 -26.00  120
  5  \w     -8.00  31.00   0.50    0.19    --   -3.12 -99.00  90.00   78
  6  \w     -7.00  30.00   0.50    0.19    --   -3.12 -99.00 -60.00   74
  7  \w    -14.00  27.00   0.50    0.19    --   -3.12 -99.00-180.00   82
  8  \w   -146.00 -89.00   0.50    0.75    --  -76.71 -99.00   0.00  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1448552000
_diffrn_orient_matrix_UB_12      -0.0535597000
_diffrn_orient_matrix_UB_13      -0.0153459000
_diffrn_orient_matrix_UB_21      0.1054026000
_diffrn_orient_matrix_UB_22      0.0105547000
_diffrn_orient_matrix_UB_23      0.0456893000
_diffrn_orient_matrix_UB_31      -0.1140545000
_diffrn_orient_matrix_UB_32      -0.0576281000
_diffrn_orient_matrix_UB_33      0.0227879000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            10408
_diffrn_reflns_theta_full        61.7282
_diffrn_reflns_theta_max         61.73
_diffrn_reflns_theta_min         2.75
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    2.333
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.4309
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1207.0272
_refine_diff_density_max         0.4551
_refine_diff_density_min         -0.8746
_refine_diff_density_rms         0.1086
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_d_res_high            0.7610
_refine_ls_d_res_low             13.9477
_refine_ls_goodness_of_fit_ref   0.9728
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    49
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9728
_refine_ls_R_factor_all          0.1394
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1267P)^2^+4.7745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2057
_refine_ls_wR_factor_ref         0.2595
_reflns_Friedel_coverage         0.759
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              31
_reflns_limit_k_min              -31
_reflns_limit_l_max              8
_reflns_limit_l_min              -8
_reflns_number_gt                2978
_reflns_number_total             5414
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            jo0c00051_si_002.cif
_cod_data_source_block           2H
_cod_depositor_comments
'Adding full bibliography for 4038227--4038237.cif.'
_cod_original_cell_volume        2658.6(15)
_cod_original_sg_symbol_Hall     ' P 2 2ab'
_cod_database_code               4038236
_chemical_oxdiff_formula         CHONS
_reflns_odcompleteness_completeness 99.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C21(H21), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C19(H19a,H19b), C18(H18a,H18b), C10(H10a,H10b), C30(H30a,H30b), C32(H32a,
 H32b), C31(H31a,H31b), C11(H11a,H11b)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C7(H7), C4(H4), C23(H23), C17(H17), C26(H26), C5(H5), C6(H6),
 C24(H24), C13(H13), C14(H14), C25(H25)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.022
_oxdiff_exptl_absorpt_empirical_full_min 0.392