An electron-deficient naphthalene diimide-based metal-organic framework for detecting electron-rich molecules through photo-/chemo-induced chromism
Gao, Bohong; Hao, Pengfei; Li, Gao-Peng; Shen, Junju; Fu, Yunlong; Dalton Transactions  (2021) –; doi:10.1039/D1DT02555D

data_7708156
_publ_section_title
;
 An electron-deficient naphthalene diimide-based metal-organic framework
 for detecting electron-rich molecules through photo-/chemo-induced
 chromism
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02555D
_journal_year                    2021
_chemical_formula_moiety         'C25 H14 N2 O6 Zn, 3(C3 H7 N O)'
_chemical_formula_sum            'C34 H35 N5 O9 Zn'
_chemical_formula_weight         723.04
_chemical_properties_physical    Light-sensitive,Photo-sensitive
_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
_audit_creation_date             2020-12-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2020-12-29 deposited with the CCDC.	2021-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.046(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4323(13)
_cell_length_b                   19.699(3)
_cell_length_c                   17.150(2)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.40
_cell_volume                     3459.1(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            50746
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.372
_diffrn_reflns_theta_min         2.242
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.673
_exptl_crystal_size_mid          0.398
_exptl_crystal_size_min          0.078
_exptl_transmission_factor_max   0.942
_exptl_transmission_factor_min   0.699
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         8609
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+1.9226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6828
_reflns_number_total             8609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02555d2.cif
_cod_data_source_block           aa
_cod_original_cell_volume        3459.1(7)
_cod_database_code               7708156
_shelx_shelxl_version_number     2014/7
_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
 N5-C33 = N5-C34 = N5-C32
 1.45 with sigma of 0.01
 O9A-C33A = O9-C33
 1.25 with sigma of 0.01
 C32-C33 = C33-C34 = C34-C32
 2.5 with sigma of 0.01
 N5A-C33A = N4-C31 = N5A-C34A = N5A-C32A
 1.45 with sigma of 0.01
 N3-C27
 1.45 with sigma of 0.01
 N5-C33 \\sim N5A-C33A
 with sigma of 0.02
 N5-C32 \\sim N5A-C32A
 with sigma of 0.02
 N5-C34 \\sim N5A-C34A
 with sigma of 0.02
 C33-C32 \\sim C33A-C32A
 with sigma of 0.04
 C33-O9 \\sim C33A-O9A
 with sigma of 0.02
 C33-C34 \\sim C33A-C34A
 with sigma of 0.04
 C32-C34 \\sim C32A-C34A
 with sigma of 0.04
 N5-O9 \\sim N5A-O9A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(C33A) \\sim Ueq, Uanis(O9A) \\sim Ueq,
Uanis(N5A) \\sim Ueq, Uanis(C32A) \\sim Ueq, Uanis(C34A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 O8, N4, C29, C30, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7, N3, C26, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O9A)=Sof(N5A)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33A)=Sof(H33A)=
 Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(O9)=Sof(N5)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33)=
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
6.a Riding coordinates:
 C32(H32A,H32B,H32C), C33(H33), C34(H34A,H34B,H34C), C32A(H32D,H32E,H32F),
 C33A(H33A), C34A(H34D,H34E,H34F)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C12(H12), C13(H13), C16(H16), C17(H17),
 C20(H20), C21(H21), C22(H22), C24(H24), C28(H28), C31(H31)
6.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C)
;
_shelx_res_checksum              32866
_shelx_hkl_checksum              53828
_olex2_submission_special_instructions 'No special instructions were received'