A donor-acceptor type macrocycle: toward photolyzable self-assembly.
Tian, Tian; Qian, Tingjuan; Jiang, Tingting; Deng, Yakui; Li, Xiaopei; Yuan, Wei; Chen, Yulan; Wang, Yi-Xuan; Hu, Wenping; Chemical communications (Cambridge, England) 56 (2020) 3939–3942; doi:10.1039/d0cc01350a

data_7126277
_publ_section_title
;
 A donor-acceptor type macrocycle: toward photolyzable self-assembly.
;
_journal_issue                   28
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3939
_journal_page_last               3942
_journal_paper_doi               10.1039/d0cc01350a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C8 H3 O6 S2, C36 H40 N2 O6'
_chemical_formula_sum            'C44 H43 N2 O12 S2'
_chemical_formula_weight         855.92
_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     dual
_audit_creation_date             2019-10-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-20 deposited with the CCDC.	2020-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                116.533(4)
_cell_angle_beta                 90.512(4)
_cell_angle_gamma                99.240(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2048(4)
_cell_length_b                   15.0598(6)
_cell_length_c                   16.5389(7)
_cell_measurement_reflns_used    7666
_cell_measurement_temperature    159.99(10)
_cell_measurement_theta_max      24.3990
_cell_measurement_theta_min      2.2170
_cell_volume                     2016.11(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      159.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.818
_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    -17.00  85.00   0.50   20.00    --    9.60  57.00 -30.00  204
  2  \w    -26.00  55.00   0.50   20.00    --    9.60 -99.00  30.00  162
  3  \w    -19.00   7.00   0.50   20.00    --  -11.16 -99.00 150.00   52
  4  \w    -66.00  37.00   0.50   20.00    --    9.60 -57.00  90.00  206
  5  \w    -45.00  64.00   0.50   20.00    --  -11.16  75.00 177.00  218
  6  \w    -86.00  23.00   0.50   20.00    --  -11.16 -75.00  49.00  218
  7  \w     -7.00  39.00   0.50   20.00    --    9.60 -99.00-180.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0588650000
_diffrn_orient_matrix_UB_12      0.0223888000
_diffrn_orient_matrix_UB_13      -0.0161577000
_diffrn_orient_matrix_UB_21      0.0489518000
_diffrn_orient_matrix_UB_22      0.0055395000
_diffrn_orient_matrix_UB_23      0.0359942000
_diffrn_orient_matrix_UB_31      0.0168886000
_diffrn_orient_matrix_UB_32      -0.0483389000
_diffrn_orient_matrix_UB_33      -0.0275812000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_unetI/netI     0.1033
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.818
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27136
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.818
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.060
_diffrn_reflns_theta_min         2.251
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43d (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             898
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         8825
_refine_ls_number_restraints     512
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1406
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0735P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4387
_reflns_number_total             8825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01350a2.cif
_cod_data_source_block           027459_tt_a
_cod_depositor_comments          'Adding full bibliography for 7126277.cif.'
_cod_original_cell_volume        2016.12(16)
_cod_database_code               7126277
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.980
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C43A-C44A
 1.5 with sigma of 0.02
 O12-C43 \\sim O12A-C43A
 with sigma of 0.02
 O12-C42 \\sim O12A-C42
 with sigma of 0.02
 O10-C44 \\sim O10-C44A
 with sigma of 0.02
 C44-C43 \\sim C44A-C43A
 with sigma of 0.02
 C42-C43 \\sim C42-C43A
 with sigma of 0.04
 O10-C43 \\sim O10-C43A
 with sigma of 0.04
 O12-C44 \\sim O12A-C44A
 with sigma of 0.04
 C42-O12 \\sim O12-C43
 with sigma of 0.02
3. Rigid bond restraints
 O10, C44, C43, O12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O10 \\sim C44 \\sim C43 \\sim O12: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.001
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(H42C)=Sof(H42D)=Sof(C44A)=Sof(H44C)=Sof(H44D)=Sof(C43A)=Sof(H43C)=
 Sof(H43D)=Sof(O12A)=1-FVAR(1)
 Sof(O12)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=
 Sof(H43B)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C26(H26A,H26B), C25(H25A,H25B), C28(H28A,H28B), C23(H23A,
 H23B), C24(H24A,H24B), C39(H39A,H39B), C44(H44A,H44B), C40(H40A,H40B),
 C41(H41A,H41B), C42(H42C,H42D), C42(H42A,H42B), C43(H43A,H43B), C44A(H44C,
 H44D), C43A(H43C,H43D)
7.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C33(H33), C12(H12), C32(H32), C11(H11), C30(H30),
 C38(H38), C9(H9), C22(H22), C35(H35), C29(H29), C19(H19), C10(H10), C37(H37),
 C20(H20), C36(H36), C21(H21)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7137
_shelx_fab_checksum              21208
_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 1.152
_oxdiff_exptl_absorpt_empirical_full_min 0.916