Integration of perylene diimide into a two-dimensional cobalt-organic framework for enhanced photocatalysis
Ma, Li-Li; Liu, Shengjin; Yang, Feinian; Cao, Jian; Ding, Longyi; Li, Yang; Yuan, Guozan; Chemical Communications  (2025) –; doi:10.1039/D5CC05626H

data_7135160
_publ_section_title
;
 Integration of perylene diimide into a two-dimensional cobalt-organic
 framework for enhanced photocatalysis
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D5CC05626H
_journal_year                    2025
_chemical_formula_moiety         'C234 H150 Co4 N6 O36, 5(C3 H7 N O), 4[C2H5O]'
_chemical_formula_sum            'C257 H205 Co4 N11 O45'
_chemical_formula_weight         4403.03
_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   mixed
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2pn3wc
_audit_creation_date             2025-09-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-09-28 deposited with the CCDC.	2025-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                77.8250(10)
_cell_angle_beta                 85.366(2)
_cell_angle_gamma                65.6610(10)
_cell_formula_units_Z            2
_cell_length_a                   22.5652(6)
_cell_length_b                   22.5982(6)
_cell_length_c                   30.2731(8)
_cell_measurement_reflns_used    9198
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      67.22
_cell_measurement_theta_min      3.34
_cell_volume                     13748.6(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            428551
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.858
_diffrn_reflns_theta_min         2.365
_exptl_absorpt_coefficient_mu    2.392
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4721
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1243 before and 0.0682 after correction.
The Ratio of minimum to maximum transmission is 0.6269.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_description       block
_exptl_crystal_F_000             4584
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.395
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2847
_refine_ls_number_reflns         50391
_refine_ls_number_restraints     11159
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1397
_refine_ls_R_factor_gt           0.1082
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+60.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2375
_refine_ls_wR_factor_ref         0.2525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32881
_reflns_number_total             50391
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05626h2.cif
_cod_data_source_block           Co-PDI
_cod_database_code               7135160
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.716
_shelx_estimated_absorpt_t_min   0.659
_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
 C249-C235
 1.53 with sigma of 0.01
 C8-C189 = C259-C15
 1.45 with sigma of 0.02
 O36-O44
 3.2 with sigma of 0.01
 C243-C236 = C232-C204 = C243-C204 = C248-C232
 1.53 with sigma of 0.01
 C204-C236
 2.55 with sigma of 0.02
 C253-O43
 1.22 with sigma of 0.02
 C256-O44
 1.22 with sigma of 0.02
 C259-O45
 1.22 with sigma of 0.02
 C259-C15
 1.36 with sigma of 0.02
 C162-C219
 1.53 with sigma of 0.01
 C219-C162
 1.53 with sigma of 0.01
 O45-C259 = O12-C189
 1.35 with sigma of 0.01
 C252-C246
 1.53 with sigma of 0.01
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C8 \\sim C15 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7
\\sim C227 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim
C257 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22
\\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30
\\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38
\\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46
\\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54
\\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62
\\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70
\\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78
\\sim C79 \\sim C80 \\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86
\\sim C87 \\sim C88 \\sim C89 \\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94
\\sim C95 \\sim C96 \\sim C97 \\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim
C102 \\sim C103 \\sim C104 \\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim
C109 \\sim C110 \\sim C111 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim
C116 \\sim C117 \\sim C118 \\sim C119 \\sim C120 \\sim C121 \\sim C122 \\sim
C123 \\sim C124 \\sim C125 \\sim C126 \\sim C127 \\sim C128 \\sim C129 \\sim
C130 \\sim C131 \\sim C132 \\sim C133 \\sim C134 \\sim C135 \\sim C136 \\sim
C137 \\sim C138 \\sim C139 \\sim C140 \\sim C141 \\sim C142 \\sim C143 \\sim
C144 \\sim C145 \\sim C146 \\sim C147 \\sim C148 \\sim C149 \\sim C150 \\sim
C151 \\sim C152 \\sim C153 \\sim C154 \\sim C155 \\sim C156 \\sim C157 \\sim
C158 \\sim C159 \\sim C160 \\sim C161 \\sim C162 \\sim C163 \\sim C164 \\sim
C165 \\sim C166 \\sim C167 \\sim C168 \\sim C169 \\sim C170 \\sim C171 \\sim
C172 \\sim C173 \\sim C174 \\sim C175 \\sim C176 \\sim C177 \\sim C178 \\sim
C179 \\sim C180 \\sim C181 \\sim C182 \\sim C183 \\sim C184 \\sim C185 \\sim
C186 \\sim C187 \\sim C188 \\sim C189 \\sim C190 \\sim C191 \\sim C192 \\sim
C193 \\sim C194 \\sim C196 \\sim C197 \\sim C198 \\sim C199 \\sim C200 \\sim
C201 \\sim C202 \\sim C203 \\sim C204 \\sim C205 \\sim C206 \\sim C207 \\sim
C208 \\sim C209 \\sim C211 \\sim C213 \\sim C214 \\sim C215 \\sim C217 \\sim
C218 \\sim C219 \\sim C222 \\sim C223 \\sim C225 \\sim C226 \\sim C230 \\sim
C231 \\sim C232 \\sim C233 \\sim C234 \\sim C235 \\sim C236 \\sim C238 \\sim
C240 \\sim C241 \\sim C242 \\sim C243 \\sim C246 \\sim C248 \\sim C249 \\sim
C252 \\sim C253 \\sim C256 \\sim C259 \\sim C195 \\sim C212 \\sim C220 \\sim
C228 \\sim C250 \\sim C251 \\sim C210 \\sim C216 \\sim C221 \\sim C224 \\sim
C229 \\sim C247 \\sim C237 \\sim C244 \\sim C245 \\sim C254 \\sim C255 \\sim N1
\\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim N10 \\sim N9 \\sim
N11 \\sim N12 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7
\\sim O8 \\sim O9 \\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15
\\sim O16 \\sim O17 \\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23
\\sim O24 \\sim O25 \\sim O26 \\sim O27 \\sim O28 \\sim O29 \\sim O30 \\sim O31
\\sim O32 \\sim O33 \\sim O38 \\sim O39 \\sim O40 \\sim O41 \\sim O43 \\sim O44
\\sim O45 \\sim O34 \\sim O35 \\sim O36 \\sim O37 \\sim O42: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
O45 \\sim C15: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(O35) \\sim Ueq, Uanis(C228) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(C250)
\\sim Ueq, Uanis(C251) \\sim Ueq, Uanis(O42) \\sim Ueq, Uanis(C244) \\sim Ueq,
Uanis(N12) \\sim Ueq, Uanis(C245) \\sim Ueq, Uanis(C237) \\sim Ueq, Uanis(C204)
\\sim Ueq, Uanis(C232) \\sim Ueq, Uanis(C248) \\sim Ueq, Uanis(C243) \\sim Ueq,
Uanis(C236) \\sim Ueq, Uanis(O45) \\sim Ueq, Uanis(C259) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C249) \\sim Ueq, Uanis(C235) \\sim Ueq, Uanis(C197) \\sim Ueq,
Uanis(C218) \\sim Ueq, Uanis(C214) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O38) \\sim Ueq, Uanis(C219) \\sim Ueq, Uanis(O39) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C255) \\sim Ueq, Uanis(C253) \\sim Ueq, Uanis(O43) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C189) = Uanis(C8)
5. Rigid body (RIGU) restrains
 O45, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Riding coordinates:
 C172(H172), C236(H23K,H23L,H23M)
6.b Ternary CH refined with riding coordinates:
 C173(H173), C187(H187), C197(H197), C204(H204), C205(H205)
6.c Secondary CH2 refined with riding coordinates:
 C189(H18A,H18B), C194(H19A,H19B), C203(H20D,H20E), C218(H21M,H21N), C223(H22D,
 H22E), C226(H22I,H22J), C230(H23A,H23B), C231(H23C,H23D), C232(H23E,H23F),
 C233(H23G,H23H), C235(H23I,H23J), C238(H23N,H23O), C243(H24D,H24E), C253(H25A,
 H25B), C256(H25C,H25D), C259(H25E,H25F)
6.d Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C255(H25J,H25K,H25L)
6.e Aromatic/amide H refined with riding coordinates:
 C7(H7), C227(H227), C28(H28), C29(H29), C33(H33), C34(H34), C36(H36),
 C38(H38), C47(H47), C49(H49), C53(H53), C55(H55), C60(H60), C68(H68), C69(H69),
  C74(H74), C80(H80), C83(H83), C85(H85), C86(H86), C90(H90), C92(H92),
 C93(H93), C95(H95), C97(H97), C98(H98), C99(H99), C103(H103), C105(H105),
 C106(H106), C107(H107), C108(H108), C110(H110), C112(H112), C118(H118),
 C119(H119), C122(H122), C123(H123), C124(H124), C125(H125), C126(H126),
 C130(H130), C132(H132), C134(H134), C136(H136), C137(H137), C138(H138),
 C139(H139), C140(H140), C141(H141), C143(H143), C144(H144), C146(H146),
 C149(H149), C150(H150), C151(H151), C153(H153), C154(H154), C156(H156),
 C157(H157), C160(H160), C161(H161), C163(H163), C166(H166), C169(H169),
 C175(H175), C179(H179), C180(H180), C184(H184), C185(H185), C188(H188),
 C190(H190), C191(H191), C192(H192), C193(H193), C199(H199), C200(H200),
 C202(H202), C206(H206), C207(H207), C208(H208), C234(H234), C241(H241),
 C242(H242), C195(H195), C228(H228), C210(H210), C224(H224), C244(H244)
6.f Naphthalene refined as free rotating group:
 C154(C155,C156,C157,C158,C159,C160,C161,C162,C163)
6.g Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C198(H19C,H19D,H19E), C201(H20A,H20B,H20C), C211(H21A,
 H21B,H21C), C213(H21D,H21E,H21F), C214(H21G,H21H,H21I), C217(H21J,H21K,H21L),
 C222(H22A,H22B,H22C), C225(H22F,H22G,H22H), C240(H24A,H24B,H24C), C248(H24F,
 H24G,H24H), C249(H24I,H24J,H24K), C212(H21O,H21P,H21Q), C220(H22K,H22L,H22M),
 C250(H25M,H25N,H25O), C251(H25P,H25Q,H25R), C216(H21R,H21S,H21T), C221(H22N,
 H22O,H22P), C229(H22Q,H22R,H22S), C247(H24L,H24M,H24N), C237(H23P,H23Q,H23R),
 C245(H24O,H24P,H24Q), C254(H25G,H25H,H25I)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1086 electrons were 
found in a volume of 4362\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
13[C3H7NO] per Unit Cell 
which account for 1040 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              47529
_shelx_hkl_checksum              5588
_shelx_fab_checksum              41310
_olex2_submission_special_instructions 'No special instructions were received'