A photochromic metal–organic framework with a rare 3D self-interpenetrated architecture and an ultrahigh MnO4− sensing ability
Zhang, Jinfang; Yue, Yinlong; Tao, Xingyu; Zhang, Jiarun; Yin, Dejing; Zhang, Chi; New Journal of Chemistry 48 (2024) 12609–12615; doi:10.1039/D4NJ02133A

data_7063269
_publ_section_title
;
 A photochromic metal--organic framework with a rare 3D
 self-interpenetrated architecture and an ultrahigh MnO4&#x2212; sensing
 ability
;
_journal_issue                   28
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12609
_journal_page_last               12615
_journal_paper_doi               10.1039/D4NJ02133A
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C64 H43 N4 Ni2 O11.5, 3.5(C3 H8 O)'
_chemical_formula_sum            'C74.5 H71 N4 Ni2 O15'
_chemical_formula_weight         1379.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-06-04
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-06-12 deposited with the CCDC.	2024-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.359(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8356(6)
_cell_length_b                   17.6855(8)
_cell_length_c                   27.7286(13)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    296.15(10)
_cell_measurement_theta_max      73.799
_cell_measurement_theta_min      2.997
_cell_volume                     7015.5(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_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  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15(10)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            78514
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.587
_diffrn_reflns_theta_min         2.996
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.227
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1082 before and 0.0654 after correction.
The Ratio of minimum to maximum transmission is 0.9021.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       block
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.00069(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1189
_refine_ls_number_reflns         14264
_refine_ls_number_restraints     1187
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1610P)^2^+1.1303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2044
_refine_ls_wR_factor_ref         0.2317
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10458
_reflns_number_total             14264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02133a2.cif
_cod_data_source_block           20230908_hg_zjf_3
_cod_depositor_comments          'Adding full bibliography for 7063269.cif.'
_cod_original_formula_sum        'C74.50 H71 N4 Ni2 O15'
_cod_database_code               7063269
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.710
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C65-C64 = C66-C64 = C72-C70 = C71-C70 = C68-C67 = C69-C67
 1.54 with sigma of 0.01
 O14-C67 = O13-C64 = O15-C70
 1.43 with sigma of 0.01
 O15A-C70A
 1.43 with sigma of 0.01
 O13-C65 = O13-C66 = O14-C69 = O14-C68 = O15-C71 = O15-C71
 2.426 with sigma of 0.02
 C71-C72 = C68-C69 = C65-C66
 2.515 with sigma of 0.02
 O11-C51 \\sim O11A-C51
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C67 \\sim C68 \\sim C69 \\sim O14 \\sim C67A \\sim C68A \\sim C69A \\sim O14A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C64 \\sim C65 \\sim C66 \\sim O13 \\sim C64A \\sim C65A \\sim C66A \\sim O13A
\\sim C64B \\sim C65B \\sim C66B \\sim O13B: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C70 \\sim C71 \\sim C72 \\sim O15 \\sim C70A \\sim C71A \\sim C72A \\sim O15A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
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 O2 \\sim O3 \\sim
O4 \\sim O5 \\sim O6 \\sim C37A \\sim C38A \\sim C39A \\sim C40A \\sim C41A
\\sim C42A \\sim C43A \\sim C44A \\sim C45A \\sim C46A \\sim C47A \\sim C48A
\\sim C49A \\sim C50A \\sim O2A \\sim O3A \\sim O4A \\sim O5A \\sim O6A \\sim
Ni2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C51 \\sim O11 \\sim O11A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(O13)
\\sim Ueq, Uanis(C64A) \\sim Ueq, Uanis(C65A) \\sim Ueq, Uanis(C66A) \\sim Ueq,
Uanis(O13A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C67) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(O14)
\\sim Ueq, Uanis(C67A) \\sim Ueq, Uanis(C68A) \\sim Ueq, Uanis(C69A) \\sim Ueq,
Uanis(O14A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(O15)
\\sim Ueq, Uanis(C70A) \\sim Ueq, Uanis(C71A) \\sim Ueq, Uanis(C72A) \\sim Ueq,
Uanis(O15A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Same fragment restrains
{Ni2, C37A, C38A, C39A, C40A, C41A, C42A, C43A, C44A, C45A, C46A, C47A, C48A,
C49A, C50A, O2A, O3A, O4A, O5A, O6A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{Ni2, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47, C48, C49, C50, O2,
O3, O4, O5, O6}
{C64A, C65A, C66A, O13A} sigma for 1-2: 0.01, 1-3: 0.02
{C64B, C65B, C66B, O13B} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C64, C65, C66, O13}
{C67A, C68A, C69A, O14A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C67, C68, C69, O14}
{C70A, C71A, C72A, O15A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C70, C71, C72, O15}
5. Others
 1*[Sof(C64)+Sof(H64)+Sof(C65)+Sof(H65A)+Sof(H65B)+Sof(H65C)+Sof(C66)+
 Sof(H66A)+Sof(H66B)+Sof(H66C)+Sof(O13)+Sof(H13)]+1*[Sof(C64A)+Sof(H64A)+
 Sof(C65A)+Sof(H65D)+Sof(H65E)+Sof(H65F)+Sof(C66A)+Sof(H66D)+Sof(H66E)+
 Sof(H66F)+Sof(O13A)+Sof(H13A)]+1*[Sof(C64B)+Sof(H64B)+Sof(C65B)+Sof(H65G)+
 Sof(H65H)+Sof(H65I)+Sof(C66B)+Sof(H66G)+Sof(H66H)+Sof(H66I)+Sof(O13B)+
 Sof(H13B)]=1.5 with esd of 0
 Sof(C38A)=Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(C42A)=
 Sof(H42A)=Sof(C43A)=Sof(H43A)=Sof(C44A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=
 Sof(H46A)=Sof(C47A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(H49A)=Sof(C50A)=Sof(O2A)=
 Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=1-FVAR(1)
 Sof(C38)=Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40)=Sof(C41)=Sof(C42)=Sof(H42)=
 Sof(C43)=Sof(H43)=Sof(C44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=
 Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=Sof(C50)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=
 Sof(O6)=FVAR(1)
 Sof(C67A)=Sof(H67A)=Sof(C68A)=Sof(H68D)=Sof(H68E)=Sof(H68F)=Sof(C69A)=
 Sof(H69D)=Sof(H69E)=Sof(H69F)=Sof(O14A)=Sof(H14B)=1-FVAR(2)
 Sof(C67)=Sof(H67)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C69)=Sof(H69A)=
 Sof(H69B)=Sof(H69C)=Sof(O14)=Sof(H14A)=FVAR(2)
 Sof(C64)=Sof(H64)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=Sof(C66)=Sof(H66A)=
 Sof(H66B)=Sof(H66C)=Sof(O13)=Sof(H13)=FVAR(3)
 Sof(C70A)=Sof(H70A)=Sof(C71A)=Sof(H71D)=Sof(H71E)=Sof(H71F)=Sof(C72A)=
 Sof(H72D)=Sof(H72E)=Sof(H72F)=Sof(O15A)=Sof(H15B)=1-FVAR(4)
 Sof(C70)=Sof(H70)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(C72)=Sof(H72A)=
 Sof(H72B)=Sof(H72C)=Sof(O15)=Sof(H15A)=FVAR(4)
 Sof(C37A)=1-FVAR(5)
 Sof(C37)=FVAR(5)
 Sof(O11A)=1-FVAR(6)
 Sof(O11)=FVAR(6)
 Sof(C64A)=Sof(H64A)=Sof(C65A)=Sof(H65D)=Sof(H65E)=Sof(H65F)=Sof(C66A)=
 Sof(H66D)=Sof(H66E)=Sof(H66F)=Sof(O13A)=Sof(H13A)=FVAR(7)
 Sof(C64B)=Sof(H64B)=Sof(C65B)=Sof(H65G)=Sof(H65H)=Sof(H65I)=Sof(C66B)=
 Sof(H66G)=Sof(H66H)=Sof(H66I)=Sof(O13B)=Sof(H13B)=FVAR(8)
 Fixed Sof: O1(0.5) H1A(0.5) H1B(0.5)
6.a Riding coordinates:
 O1(H1A,H1B), O12(H12A,H12B), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C),
 O13(H13), O14(H14A), O15(H15A), C65A(H65D,H65E,H65F), O13A(H13A), O14A(H14B),
 C72A(H72D,H72E,H72F), C65B(H65G,H65H,H65I), C66B(H66G,H66H,H66I), O13B(H13B)
6.b Ternary CH refined with riding coordinates:
 C64(H64), C67(H67), C70(H70), C64A(H64A), C67A(H67A), C70A(H70A), C64B(H64B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C21(H21), C22(H22), C23(H23), C24(H24), C28(H28),
  C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36),
 C53(H53), C54(H54), C56(H56), C57(H57), C59(H59), C60(H60), C62(H62), C63(H63),
  C39(H39), C40(H40), C42(H42), C43(H43), C45(H45), C46(H46), C48(H48),
 C49(H49), C39A(H39A), C40A(H40A), C42A(H42A), C43A(H43A), C45A(H45A),
 C46A(H46A), C48A(H48A), C49A(H49A)
6.d Idealised Me refined as rotating group:
 C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C72(H72A,H72B,
 H72C), C66A(H66D,H66E,H66F), C68A(H68D,H68E,H68F), C69A(H69D,H69E,H69F),
 C71A(H71D,H71E,H71F)
6.e Idealised tetrahedral OH refined as rotating group:
 O15A(H15B)
;
_shelx_res_checksum              43361
_shelx_hkl_checksum              66014
_olex2_submission_special_instructions 'No special instructions were received'