Coordination-driven self-assembly of anthraquinone-based metal-organic cages for photocatalytic selective [2 + 2] cycloaddition.
Jin, Yao; Jiang, Hong; Tang, Xianhui; Zhang, Wenqiang; Liu, Yan; Cui, Yong; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8533–8539; doi:10.1039/d1dt00652e

data_7707521
_publ_section_title
;
 Coordination-driven self-assembly of anthraquinone-based metal-organic
 cages for photocatalytic selective [2 + 2] cycloaddition.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8533
_journal_page_last               8539
_journal_paper_doi               10.1039/d1dt00652e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C288 H224 Co16 O100 S16'
_chemical_formula_sum            'C288 H224 Co16 O100 S16'
_chemical_formula_weight         6740.50
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc27rnzn
_audit_creation_date             2021-05-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-21 deposited with the CCDC.	2021-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   31.0736(6)
_cell_length_b                   31.0736(6)
_cell_length_c                   25.0692(10)
_cell_measurement_reflns_used    9399
_cell_measurement_temperature    173
_cell_measurement_theta_max      59.035
_cell_measurement_theta_min      2.264
_cell_volume                     24206.0(12)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1236
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            133041
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        59.074
_diffrn_reflns_theta_max         59.074
_diffrn_reflns_theta_min         2.264
_diffrn_source_current           45.0
_diffrn_source_power             2.25
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    5.274
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.4559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1348 before and 0.0882 after correction.
The Ratio of minimum to maximum transmission is 0.6066.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear pinkish pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    0.925
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             6880
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         8771
_refine_ls_number_restraints     1127
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1283
_refine_ls_R_factor_gt           0.0924
_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^)+(0.1331P)^2^+247.6790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2524
_refine_ls_wR_factor_ref         0.2853
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6392
_reflns_number_total             8771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00652e2.cif
_cod_data_source_block           2-Co
_cod_depositor_comments
'Adding full bibliography for 7707521--7707522.cif.'
_cod_original_cell_volume        24206.0(13)
_cod_database_code               7707521
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C34A-C33 = C36-C33 = C34-C33 = C36A-C33 = C35-C33 = C33-C35A
 1.51 with sigma of 0.02
 C32-C33A = C32-C33
 1.51 with sigma of 0.02
 C33A-C35A = C33A-C36A = C34A-C33A
 1.51 with sigma of 0.02
 C23A-C24 = C23A-C24A = C23A-C26 = C23A-C26A = C23A-C25 = C23A-C25A
 1.51 with sigma of 0.02
 C23-C26 = C23-C24 = C23-C25
 1.51 with sigma of 0.02
 C36-C33 = C34-C33 = C35-C33 = C23A-C26A = C23A-C24A = C23A-C25A
 1.51 with sigma of 0.02
 C34A-C33A = C33A-C35A = C33A-C36A = C23-C26 = C23-C24 = C23-C25
 1.51 with sigma of 0.02
 C36-C32 \\sim C32-C35
 with sigma of 0.02
 C34A-C36A \\sim C36A-C35A
 with sigma of 0.02
 C36-C34 \\sim C34-C35
 with sigma of 0.02
 C34-C35 \\sim C35-C36
 with sigma of 0.02
 C36-C32 \\sim C32-C34
 with sigma of 0.02
 C35A-C34A \\sim C34A-C36A
 with sigma of 0.02
 C36A-C35A \\sim C35A-C34A
 with sigma of 0.02
 C25A-C26A \\sim C26A-C24A
 with sigma of 0.02
 C24A-C25A \\sim C25A-C26A
 with sigma of 0.02
 C25-C24 \\sim C24-C26
 with sigma of 0.02
 C26-C25 \\sim C25-C24
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C23A)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C26A)=Sof(H26D)=
 Sof(H26E)=Sof(H26F)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C23)=FVAR(1)
 Sof(C33)=Sof(C36)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C34)=Sof(H34D)=Sof(H34E)=
 Sof(H34F)=Sof(C35)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(2)
 Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C34A)=Sof(H34A)=Sof(H34B)=
 Sof(H34C)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C33A)=FVAR(2)
6.a Me refined with riding coordinates:
 C35A(H35A,H35B,H35C), C34A(H34A,H34B,H34C), C36A(H36A,H36B,H36C), C24(H24A,
 H24B,H24C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C24A(H24D,H24E,H24F),
 C26A(H26D,H26E,H26F), C25A(H25D,H25E,H25F), C36(H36D,H36E,H36F), C34(H34D,H34E,
 H34F), C35(H35D,H35E,H35F)
6.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C27(H27), C19(H19), C21(H21), C4(H4), C3(H3), C7(H7), C15(H15),
 C13(H13), C12(H12)
6.c Fitted hexagon refined as free rotating group:
 C29(C30,C31,C32,C27,C28), C17(C18,C19,C20,C21,C22), C5(C4,C3,C2,C7,C6),
 C10(C9,C15,C14,C13,C12)
;
_shelx_res_checksum              34780
_shelx_hkl_checksum              7153
_shelx_fab_checksum              20837
_olex2_submission_special_instructions 'No special instructions were received'