Porous MOFs with geometric mismatch between trimers and octatopic pyrene-based ligands for low-temperature methane storage.
Wang, Kun; Cao, Honghao; Zhong, Yuanlong; Yang, Zhenning; Shi, Hancheng; Xiong, Zhangyi; Mu, Yuqiao; Chen, Zhijie; Chemical communications (Cambridge, England) 60 (2024) 15055–15058; doi:10.1039/d4cc04907a

data_7134009
_publ_section_title
;
 Porous MOFs with geometric mismatch between trimers and octatopic
 pyrene-based ligands for low-temperature methane storage.
;
_journal_issue                   100
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              15055
_journal_page_last               15058
_journal_paper_doi               10.1039/d4cc04907a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C192 H100 Fe6 O38'
_chemical_formula_sum            'C192 H100 Fe6 O38'
_chemical_formula_weight         3349.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-31
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-19 deposited with the CCDC.	2024-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.444(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   27.880(9)
_cell_length_b                   19.220(7)
_cell_length_c                   40.725(15)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    273.0
_cell_measurement_theta_max      18.15
_cell_measurement_theta_min      2.20
_cell_volume                     21757(13)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68883
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.1072
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            47573
_diffrn_reflns_point_group_measured_fraction_full 0.898
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        18.870
_diffrn_reflns_theta_max         18.870
_diffrn_reflns_theta_min         0.855
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_T_max  0.7442
_exptl_absorpt_correction_T_min  0.4981
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0999 before and 0.0674 after correction.
The Ratio of minimum to maximum transmission is 0.6693.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.511
_exptl_crystal_description       prism
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.479(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1754
_refine_ls_number_reflns         30836
_refine_ls_number_restraints     1875
_refine_ls_restrained_S_all      3.669
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0406P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1226
_reflns_Friedel_coverage         0.761
_reflns_Friedel_fraction_full    0.811
_reflns_Friedel_fraction_max     0.811
_reflns_number_gt                21940
_reflns_number_total             30836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04907a2.cif
_cod_data_source_block           Fe_TPBB
_cod_depositor_comments
'Adding full bibliography for 7134009--7134010.cif.'
_cod_database_code               7134009
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.989
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.52112
 0.47888
2. Restrained distances
 C72-C75
 1.4 with sigma of 0.02
 C118-O16
 1.2 with sigma of 0.02
 O17-C118 = O16-C118
 1.2 with sigma of 0.02
 O16-O17
 2.1 with sigma of 0.02
 O17-C115
 2.3 with sigma of 0.02
 C22-C76
 1.5 with sigma of 0.001
 C23-C26
 1.5 with sigma of 0.001
 C118-C115
 1.5 with sigma of 0.001
 C57-C33
 1.5 with sigma of 0.001
 C35-C36
 1.5 with sigma of 0.001
 Fe5-C88 = C88-C80
 1.4 with sigma of 0.02
 C141-C136 = C138-C139 = C139-C140
 1.37 with sigma of 0.02
 C111-C112
 2.3 with sigma of 0.02
 C111-C103
 2.3 with sigma of 0.02
 C141-C140
 1.38 with sigma of 0.02
 C136-C137 = C137-C138
 1.36 with sigma of 0.02
 C134-C136
 1.4 with sigma of 0.02
 C173-C151
 1.4 with sigma of 0.02
 C56-C44
 1.5 with sigma of 0.001
 C17-C19
 1.5 with sigma of 0.001
 C183-C186
 1.5 with sigma of 0.001
 C1-C2
 1.5 with sigma of 0.001
 C5-C8
 1.5 with sigma of 0.001
 C103-C106
 1.5 with sigma of 0.001
 C192-C108
 1.5 with sigma of 0.001
 C112-C110
 1.5 with sigma of 0.001
 C154-C145
 1.5 with sigma of 0.001
 C143-C127
 1.5 with sigma of 0.001
 C130-C129
 1.5 with sigma of 0.001
 C190-C119
 1.5 with sigma of 0.001
 C69-C59
 1.5 with sigma of 0.001
 C75-C72
 1.5 with sigma of 0.001
 C63-C61
 1.5 with sigma of 0.001
 C88-C80
 1.5 with sigma of 0.001
 C14-C12
 1.5 with sigma of 0.001
 C47-C38
 1.5 with sigma of 0.001
 C20-C10
 1.5 with sigma of 0.001
 C120-C170
 1.5 with sigma of 0.001
 C121-C120
 1.5 with sigma of 0.001
 C167-C132
 1.5 with sigma of 0.001
 C180-C98_$1
 1.5 with sigma of 0.001
 C78-C82
 1.5 with sigma of 0.001
 C141-C137 = C137-C139 = C138-C140
 2.37 with sigma of 0.04
 C141-C139
 2.38 with sigma of 0.04
 C136-C138
 2.36 with sigma of 0.04
 C118-O16 \\sim C118-O17
 with sigma of 0.02
 C116-C118 \\sim C118-C114
 with sigma of 0.02
 C141-C136 \\sim C136-C137 \\sim C137-C138 \\sim C138-C139 \\sim C139-C140
\\sim C140-C141
 with sigma of 0.02
 C141-C139 \\sim C141-C137 \\sim C139-C137 \\sim C138-C136 \\sim C138-C140
\\sim C140-C136
 with sigma of 0.04
 C112-C111 \\sim C112-C109
 with sigma of 0.02
3. Restrained planarity
 C118, C115, O17, O16
 with sigma of 0.01
 C118, C114, C115, C116
 with sigma of 0.1
 C114, C115, C116, C118
 with sigma of 0.01
 C141, C136, C137, C138, C139, C140
 with sigma of 0.1
 C173, C151, O1, O15A
 with sigma of 0.1
 C113, C112, C117, C110
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.003 and sigma
for terminal atoms of 0.006 within 2A
O33 \\sim O28 \\sim O25 \\sim O11 \\sim O6 \\sim O32 \\sim O24 \\sim O29 \\sim
O5 \\sim O14 \\sim O9 \\sim O12 \\sim O34 \\sim O15 \\sim O26 \\sim O36 \\sim
O16 \\sim O31 \\sim O19 \\sim O10 \\sim O18 \\sim O30 \\sim O8 \\sim O4 \\sim
O22 \\sim O13 \\sim O27 \\sim O35 \\sim O23 \\sim O37 \\sim O20 \\sim O2 \\sim
O7: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within
2A
O33 \\sim O16 \\sim O4 \\sim O11 \\sim O6 \\sim O32 \\sim O26 \\sim O29 \\sim
O5 \\sim O14 \\sim O9 \\sim O12 \\sim O24 \\sim O15 \\sim O28 \\sim O36 \\sim
O1 \\sim O31 \\sim O19 \\sim O10 \\sim O18 \\sim O30 \\sim O25 \\sim O8 \\sim
O34 \\sim O22 \\sim O27 \\sim O13 \\sim O23 \\sim O35 \\sim O20 \\sim O37 \\sim
O17 \\sim O2 \\sim O15A \\sim O7: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C85 \\sim C94 \\sim C52 \\sim C86 \\sim C36 \\sim C87 \\sim C180 \\sim C82
\\sim C11 \\sim C83 \\sim C112 \\sim C84 \\sim C67 \\sim C104 \\sim C34 \\sim
C103 \\sim C131 \\sim C102 \\sim C46 \\sim C101 \\sim C123 \\sim C100 \\sim
C141 \\sim C105 \\sim C56 \\sim C169 \\sim C32 \\sim C164 \\sim C28 \\sim C165
\\sim C125 \\sim C166 \\sim C133 \\sim C167 \\sim C91 \\sim C168 \\sim C9 \\sim
C190 \\sim C38 \\sim C191 \\sim C186 \\sim C114 \\sim C187 \\sim C179 \\sim
C188 \\sim C139 \\sim C189 \\sim C48 \\sim C73 \\sim C63 \\sim C72 \\sim C65
\\sim C71 \\sim C184 \\sim C70 \\sim C182 \\sim C69 \\sim C30 \\sim C74 \\sim
C120 \\sim C81 \\sim C170 \\sim C76 \\sim C171 \\sim C77 \\sim C135 \\sim C78
\\sim C89 \\sim C79 \\sim C93 \\sim C80 \\sim C13 \\sim C144 \\sim C42 \\sim
C145 \\sim C44 \\sim C146 \\sim C40 \\sim C147 \\sim C75 \\sim C142 \\sim C129
\\sim C143 \\sim C127 \\sim C155 \\sim C116 \\sim C156 \\sim C175 \\sim C157
\\sim C177 \\sim C158 \\sim C137 \\sim C159 \\sim C118 \\sim C154 \\sim C47
\\sim C110 \\sim C49 \\sim C109 \\sim C31 \\sim C108 \\sim C68 \\sim C107 \\sim
C66 \\sim C106 \\sim C64 \\sim C111 \\sim C183 \\sim C62 \\sim C185 \\sim C57
\\sim C181 \\sim C58 \\sim C33 \\sim C59 \\sim C29 \\sim C60 \\sim C35 \\sim
C61 \\sim C126 \\sim C1 \\sim C121 \\sim C96 \\sim C98 \\sim C150 \\sim C172
\\sim C151 \\sim C119 \\sim C152 \\sim C192 \\sim C153 \\sim C134 \\sim C148
\\sim C130 \\sim C149 \\sim C132 \\sim C5 \\sim C90 \\sim C4 \\sim C92 \\sim C3
\\sim C88 \\sim C2 \\sim C12 \\sim C7 \\sim C8 \\sim C6 \\sim C10 \\sim C163
\\sim C41 \\sim C54 \\sim C45 \\sim C18 \\sim C43 \\sim C17 \\sim C39 \\sim C16
\\sim C55 \\sim C15 \\sim C37 \\sim C14 \\sim C162 \\sim C95 \\sim C128 \\sim
C19 \\sim C124 \\sim C99 \\sim C122 \\sim C27 \\sim C113 \\sim C26 \\sim C115
\\sim C24 \\sim C117 \\sim C23 \\sim C97 \\sim C22 \\sim C174 \\sim C21 \\sim
C178 \\sim C20 \\sim C176 \\sim C25 \\sim C136 \\sim C53 \\sim C138 \\sim C160
\\sim C140 \\sim C50 \\sim C51: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C86 \\sim C87 \\sim C85: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C89 \\sim C88 \\sim C90: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C175 \\sim C176 \\sim C174: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C95 \\sim C85 \\sim C84 \\sim C86: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C99 \\sim C100 \\sim C105 \\sim C101: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C121 \\sim C122 \\sim C123 \\sim C172: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C123 \\sim C172 \\sim C94 \\sim C126 \\sim C125 \\sim C124: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C127 \\sim C128 \\sim C129 \\sim C124: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
C145 \\sim C144 \\sim C143 \\sim C142 \\sim C147 \\sim C146: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C191 \\sim C190 \\sim C189 \\sim C186 \\sim C187 \\sim C188: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C184 \\sim C185 \\sim C180 \\sim C181 \\sim C182: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C158 \\sim C157 \\sim C156 \\sim C154 \\sim C159: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
O29 \\sim O7 \\sim O13 \\sim O11 \\sim O4 \\sim O35 \\sim O36 \\sim O22: within
2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Uanis(O6) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O4) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(O36) \\sim Ueq, Uanis(O11)
\\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(O35) \\sim Ueq,
Uanis(O13) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O20)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O24) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
Uanis(O12) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
Uanis(O34) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C90) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C88)
\\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C76) \\sim Ueq,
Uanis(C77) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C79) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C85) \\sim Ueq, Uanis(C95) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O13) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O23) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C98) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O35) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O11) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O20) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O15) \\sim Ueq, Uanis(O14) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 C141, C136, C137, C138, C139, C140
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed U11: C118(0.058594) O16(0.059685) O17(0.059529) C161(0.05454)
 O21(0.055943) O3(0.057035)
 Fixed U22: C118(0.051) O16(0.051) O17(0.051) C161(0.051) O21(0.051) O3(0.051)
 Fixed U33: C118(0.052) O16(0.052) O17(0.052) C161(0.052) O21(0.052) O3(0.052)
 Fixed X: C118(0.40889) O16(0.42113) O17(0.3743) C161(0.68473) O21(0.72224)
 O3(0.67912)
 Fixed Y: C118(-0.921431) O16(-0.96238) O17(-0.94502) C161(0.12771)
 O21(0.10531) O3(0.17952)
 Fixed Z: C118(0.244049) O16(0.265281) O17(0.22846) C161(0.25406)
 O21(0.252439) O3(0.244289)
7.a Aromatic/amide H refined with riding coordinates:
 C86(H86), C87(H87), C83(H83), C84(H84), C104(H104), C105(H105), C101(H101),
 C102(H102), C169(H169), C165(H165), C166(H166), C168(H168), C191(H191),
 C187(H187), C189(H189), C73(H73), C71(H71), C70(H70), C74(H74), C81(H81),
 C77(H77), C79(H79), C144(H144), C146(H146), C142(H142), C155(H155), C156(H156),
  C158(H158), C159(H159), C111(H111), C107(H107), C109(H109), C62(H62),
 C58(H58), C60(H60), C150(H150), C152(H152), C153(H153), C149(H149), C4(H4),
 C3(H3), C7(H7), C6(H6), C54(H54), C18(H18), C16(H16), C15(H15), C27(H27),
 C26(H26), C21(H21), C51(H51), C52(H52), C48(H48), C49(H49), C31(H31), C68(H68),
  C67(H67), C65(H65), C64(H64), C32(H32), C184(H184), C185(H185), C181(H181),
 C182(H182), C34(H34), C126(H126), C120(H120), C121(H121), C125(H125),
 C171(H171), C133(H133), C135(H135), C131(H131), C89(H89), C90(H90), C92(H92),
 C93(H93), C11(H11), C9(H9), C13(H13), C42(H42), C46(H46), C45(H45), C43(H43),
 C39(H39), C55(H55), C37(H37), C128(H128), C113(H113), C114(H114), C116(H116),
 C117(H117), C175(H175), C179(H179), C178(H178), C176(H176), C138(H138),
 C137(H137), C141(H141), C140(H140)
7.b Fitted hexagon refined as free rotating group:
 C85(C86,C87,C82,C83,C84), C104(C105,C100,C101,C102,C103), C169(C164,C165,C166,
 C167,C168), C190(C191,C186,C187,C188,C189), C73(C72,C71,C70,C69,C74), C81(C76,
 C77,C78,C79,C80), C144(C145,C146,C147,C142,C143), C155(C156,C157,C158,C159,
 C154), C110(C111,C106,C107,C108,C109), C62(C57,C58,C59,C60,C61), C150(C151,
 C152,C153,C148,C149), C5(C4,C3,C2,C7,C6), C54(C18,C17,C16,C15,C14), C24(C23,
 C22,C21,C20,C25), C50(C51,C52,C47,C48,C49), C63(C68,C67,C66,C65,C64),
 C183(C184,C185,C180,C181,C182), C33(C28,C29,C30,C35,C34), C170(C172,C94,C119,
 C171,C192), C133(C134,C135,C130,C131,C132), C89(C90,C91,C92,C93,C88), C11(C10,
 C9,C8,C13,C12), C42(C41,C46,C45,C44,C43), C38(C39,C40,C55,C36,C37), C128(C129,
 C124,C123,C122,C127), C113(C114,C115,C116,C117,C112), C175(C174,C179,C178,C177,
 C176), C139(C138,C137,C136,C141,C140)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              39868
_shelx_hkl_checksum              86191
_shelx_fab_checksum              30000
_olex2_submission_special_instructions 'No special instructions were received'