A copper-seamed coordination nanocapsule as a semiconductor photocatalyst for molecular oxygen activation.
Hu, Xiangquan; Han, Meirong; Wang, Leicheng; Shao, Li; Peeyush, Yadav; Du, Jialei; Kelley, Steven P.; Dalgarno, Scott J.; Atwood, David A.; Feng, Sisi; Atwood, Jerry L.; Chemical science 14 (2023) 4532–4537; doi:10.1039/d3sc00318c

data_1568681
_publ_section_title
;
 A copper-seamed coordination nanocapsule as a semiconductor photocatalyst
 for molecular oxygen activation.
;
_journal_issue                   17
_journal_name_full               'Chemical science'
_journal_page_first              4532
_journal_page_last               4537
_journal_paper_doi               10.1039/d3sc00318c
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety
'C320 H407 Br3 Cu24 N8 O86, 2(H2 O), 2(C3 H7 N O)'
_chemical_formula_sum            'C326 H425 Br3 Cu24 N10 O90'
_chemical_formula_weight         7688.42
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_audit_creation_date             2021-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-20 deposited with the CCDC.	2023-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                108.799(5)
_cell_angle_beta                 106.390(5)
_cell_angle_gamma                104.441(5)
_cell_formula_units_Z            1
_cell_length_a                   22.579(8)
_cell_length_b                   22.754(8)
_cell_length_c                   24.113(8)
_cell_measurement_reflns_used    7350
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      18.64
_cell_measurement_theta_min      2.18
_cell_volume                     10431(6)
_computing_cell_refinement       'Bruker Apex3 V.2016.9-0/SAINT V8.37A'
_computing_data_collection       'Bruker Apex3 V.2016.9-0'
_computing_data_reduction        'Bruker Apex3 V.2016.9-0/SAINT V8.37A'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1828
_diffrn_reflns_av_unetI/netI     0.1914
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            82759
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        21.118
_diffrn_reflns_theta_max         21.118
_diffrn_reflns_theta_min         1.092
_diffrn_source                   'Sealed Source Mo with TRIUMPH optics'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.548
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.4487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3972
_exptl_crystal_recrystallization_method
'Spontaneously from reaction in DMF/MeOH/pyridine'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.473
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1896
_refine_ls_number_reflns         22443
_refine_ls_number_restraints     1892
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.2263
_refine_ls_R_factor_gt           0.1196
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3193
_refine_ls_wR_factor_ref         0.3859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10052
_reflns_number_total             22443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00318c2.cif
_cod_data_source_block           s1_sq
_cod_depositor_comments          'Adding full bibliography for 1568681.cif.'
_cod_database_code               1568681
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.563
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C129-C128 = C127-C128 = C127-C126 = C143-C142 = C142-C141 = C140-C141 = C133-
 C132 = C132-C131 = C131-C130 = C85-C84 = C84-C83 = C82-C83 = C91-C90 = C89-C90
 = C89-C88
 1.54 with sigma of 0.02
 C86-C85
 1.54 with sigma of 0.02
 C134-C133 = C144-C143
 1.54 with sigma of 0.02
 C39-C21
 1.54 with sigma of 0.02
 C33-C32 = C31-C32 = C31-C30
 1.54 with sigma of 0.02
 N3-C0AA \\sim N3-C157 \\sim N1-C149 \\sim N1-C145
 with sigma of 0.02
 C157-C156 \\sim C156-C2AA \\sim C2AA-C1AA \\sim C0AA-C1AA
 with sigma of 0.02
 O1S-C1S \\sim O41-C153 \\sim O37_$1-C150_$1
 with sigma of 0.02
 N1S-C3S \\sim N1S-C2S \\sim N02J-C154 \\sim N02J-C155 \\sim N2_$1-C151_$1
\\sim N2_$1-C152_$1
 with sigma of 0.02
 N1S-C1S \\sim N2_$1-C150_$1
 with sigma of 0.02
 C148-C147 \\sim C147-C146 \\sim C146-C145 \\sim C148-C149
 with sigma of 0.02
 C149-C147 \\sim C145-C148 \\sim C148-C146 \\sim C147-C145
 with sigma of 0.02
3. Restrained planarity
 Cu3, N3, C0AA, C1AA, C156, C2AA, C157
 with sigma of 0.1
 Cu1, C145, N1, C149, C146
 with sigma of 0.1
 C147, C146, N1, C148, C149, C145
 with sigma of 0.1
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
 Fixed Sof: Br5(0.3) Br4(0.3) Br2(0.3) Br3(0.3) Br1(0.3) C43(0.6) C40'(0.6)
 C40(0.6) C42(0.6) C41'(0.6)
6.a Ternary CH refined with riding coordinates:
 C103(H103), C124(H124), C28(H28), C117(H117), C14(H14), C7(H7), C55(H55),
 C110(H110), C69(H69), C21(H21), C62(H62), C76(H76)
6.b Secondary CH2 refined with riding coordinates:
 C125(H12A,H12B), C126(H12C,H12D), C92(H92A,H92B), C130(H13A,H13B), C141(H14A,
 H14B), C140(H14C,H14D), C34(H34A,H34B), C44(H44A,H44B), C87(H87A,H87B),
 C128(H12E,H12F), C29(H29A,H29B), C127(H12G,H12H), C131(H13C,H13D), C88(H88A,
 H88B), C83(H83A,H83B), C93(H93A,H93B), C142(H14E,H14F), C82(H82A,H82B),
 C132(H13E,H13F), C45(H45A,H45B), C143(H14G,H14H), C84(H84A,H84B), C30(H30A,
 H30B), C46(H46A,H46B), C90(H90A,H90B), C89(H89A,H89B), C133(H13G,H13H),
 C47(H47A,H47B), C94(H94A,H94B), C95(H95A,H95B), C85(H85A,H85B), C36(H36A,H36B),
  C35(H35A,H35B)
6.c Me refined with riding coordinates:
 C129(H12I,H12J,H12K), C155(H15A,H15B,H15C), C154(H15D,H15E,H15F), C3S(H3SA,
 H3SB,H3SC), C2S(H2SA,H2SB,H2SC), C91(H91A,H91B,H91C), C48(H48A,H48B,H48C),
 C151(H15G,H15H,H15I), C152(H15J,H15K,H15L), C86(H86A,H86B,H86C), C134(H13I,
 H13J,H13K), C144(H14I,H14J,H14K), C96(H96A,H96B,H96C)
6.d Aromatic/amide H refined with riding coordinates:
 C109(H109), C116(H116), C13(H13), C75(H75), C53(H53), C123(H123), C61(H61),
 C5(H5), C101(H101), C153(H153), C68(H68), C20(H20), C1AA(H1AA), C27(H27),
 C2AA(H2AA), C156(H156), C0AA(H0AA), C1S(H1S), C157(H157), C146(H146),
 C150(H150), C145(H145), C149(H149), C148(H148), C147(H147)
;
_shelx_res_checksum              42173
_shelx_hkl_checksum              61909
_shelx_fab_checksum              33381
_olex2_submission_special_instructions 'No special instructions were received'