Tetraphenylpyrazine-Based Luminescent Metal-Organic Framework for Chemical Sensing of Carcinoids Biomarkers.
Ying, Xu-Dong; Chen, Jian-Xiang; Tu, Dan-Yu; Zhuang, Yi-Cao; Wu, Di; Shen, Liang; ACS applied materials & interfaces 13 (2021) 6421–6429; doi:10.1021/acsami.0c20893

data_4518516
_publ_section_title
;
 Tetraphenylpyrazine-Based Luminescent Metal-Organic Framework for
 Chemical Sensing of Carcinoids Biomarkers.
;
_journal_issue                   5
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              6421
_journal_page_last               6429
_journal_paper_doi               10.1021/acsami.0c20893
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         'C48 H28 N3 O12 Zn3'
_chemical_formula_sum            'C48 H28 N3 O12 Zn3'
_chemical_formula_weight         1034.84
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.0880(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.3137(13)
_cell_length_b                   20.2338(9)
_cell_length_c                   18.0946(8)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.41
_cell_volume                     10206.0(8)
_computing_cell_refinement       'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_computing_data_reduction        'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            75257
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.385
_diffrn_reflns_theta_min         2.245
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1705 before and 0.0496 after correction.
The Ratio of minimum to maximum transmission is 0.7454.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.673
_exptl_crystal_description       block
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         20142
_refine_ls_number_restraints     1747
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0499
_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^)+(0.1021P)^2^+2.4532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14724
_reflns_number_total             20142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am0c20893_si_002.cif
_cod_data_source_block           zz_sq
_cod_database_code               4518516
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.892
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N1-C26 \\sim N1-C29 \\sim N1-C31 \\sim N1-C33
 with sigma of 0.02
 C30-C31 \\sim C32-C33 \\sim C26-C27 \\sim C28-C29 \\sim C27-C34 \\sim C28-C34
\\sim C30-C34 \\sim C32-C34
 with sigma of 0.02
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
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C45) \\sim Ueq,
Uanis(C44) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(N2) \\sim Ueq,
Uanis(C48) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C01A)
\\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
5. 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
6. Others
 Fixed Sof: C31(0.7) H31(0.7) C29(0.7) H29(0.7) C44(0.7) H44(0.7) C53(0.7)
 H53(0.7) C54(0.7) H54(0.7) C28(0.7) H28(0.7) C52(0.7) H52(0.7) C50(0.7)
 H50(0.7) C30(0.7) H30(0.7) C45(0.7) H45(0.7) C36(0.7) H36(0.7) C37(0.7)
 H37(0.7) C26(0.3) H26(0.3) C33(0.3) H33(0.3) C32(0.3) H32(0.3) C27(0.3)
 H27(0.3) C51(0.3) H51(0.3) C49(0.3) H49(0.3) C55(0.3) H55(0.3) C56(0.3)
 H56(0.3) C42(0.3) H42(0.3) C41(0.3) H41(0.3) C38(0.3) H38(0.3) C39(0.3)
 H39(0.3)
7.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C15(H15), C3(H3), C22(H22), C14(H14), C23(H23), C11(H11), C8(H8),
 C7(H7), C12(H12), C19(H19), C59(H59), C60(H60), C58(H58), C20(H20), C61(H61),
 C31(H31), C29(H29), C44(H44), C53(H53), C54(H54), C28(H28), C52(H52), C50(H50),
  C30(H30), C45(H45), C36(H36), C37(H37), C26(H26), C33(H33), C32(H32),
 C27(H27), C51(H51), C49(H49), C55(H55), C56(H56), C42(H42), C41(H41), C38(H38),
  C39(H39)
;
_shelx_res_checksum              85981
_shelx_hkl_checksum              89200
_shelx_fab_checksum              85323
_olex2_submission_special_instructions 'No special instructions were received'