Two novel zinc-based MOFs as luminescence sensors to detect phenylglyoxylic acid
Song, Dongxue; Ji, Xiaoxi; Li, Yong; Wu, Shuangyan; Zhang, Ying; Wang, Xiaofeng; Sun, Yaguang; Gao, Enjun; Zhu, Mingchang; Dalton Transactions  (2022) –; doi:10.1039/D2DT02406C

data_7711465
_publ_section_title
;
 Two novel zinc-based MOFs as luminescence sensors to detect
 phenylglyoxylic acid
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02406C
_journal_year                    2022
_chemical_formula_moiety         'C50 H44 N6 O21 Zn4'
_chemical_formula_sum            'C74 H100 N14 O29 Zn4'
_chemical_formula_weight         1911.15
_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             2022-09-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2022-09-26 deposited with the CCDC.	2022-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.529(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4312(3)
_cell_length_b                   21.5199(3)
_cell_length_c                   25.8251(5)
_cell_measurement_reflns_used    21036
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      67.9790
_cell_measurement_theta_min      2.5780
_cell_volume                     9653.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_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_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     55.00  91.00   0.50    1.18    --   42.10  68.00   6.00   72
  2  \w     20.00  51.00   0.50    1.18    --   42.10  68.00   6.00   62
  3  \w     47.00  75.00   0.50    4.73    --   94.70 -68.00-126.00   56
  4  \w     71.00 182.00   0.50    4.73    --   94.70  68.00   6.00  222
  5  \w    106.00 132.00   0.50    1.18    --   42.10  82.00  90.00   52
  6  \w     24.00 132.00   0.50    1.18    --   42.10  77.00  30.00  216
  7  \w     24.00  64.00   0.50    1.18    --   42.10 -77.00 -60.00   80
  8  \w     60.00 117.00   0.50    1.18    --   42.10  77.00 120.00  114
  9  \w     21.00  59.00   0.50    1.18    --   42.10 -32.00-120.00   76
 10  \w     13.00  45.00   0.50    1.18    --   42.10 -68.00-126.00   64
 11  \w    107.00 132.00   0.50    1.18    --   42.10  68.00   6.00   50
 12  \w    -46.00  42.00   0.50    1.18    --   42.10 -65.00 150.00  176
 13  \w     22.00  47.00   0.50    1.18    --   42.10  77.00 120.00   50
 14  \w    -31.00   8.00   0.50    1.18    --   42.10 -77.00 -60.00   78
 15  \w    -36.00 -11.00   0.50    1.18    --   42.10 -32.00-120.00   50
 16  \w     67.00  94.00   0.50    1.18    --   42.10  82.00  90.00   54
 17  \w    -35.00  55.00   0.50    1.18    --   42.10 -77.00 150.00  180
 18  \w     58.00  83.00   0.50    1.18    --   42.10  65.00-150.00   50
 19  \w     43.00 119.00   0.50    4.73    --   94.70 -68.00 -90.00  152
 20  \w      5.00  37.00   0.50    4.73    --   94.70 -68.00 -90.00   64
 21  \w     70.00 120.00   0.50    4.73    --   94.70  68.00 -30.00  100
 22  \w     12.00 125.00   0.50    4.73    --   94.70 -50.00  90.00  226
 23  \w      5.00 109.00   0.50    4.73    --   94.70 -82.00  60.00  208
 24  \w    106.00 132.00   0.50    4.73    --   94.70  68.00  90.00   52
 25  \w     71.00  96.00   0.50    4.73    --   94.70  68.00  90.00   50
 26  \w     60.00 144.00   0.50    4.73    --   94.70  33.00  90.00  168
 27  \w    102.00 184.00   0.50    4.73    --   94.70 -17.00 150.00  164
 28  \w     67.00  93.00   0.50    4.73    --   94.70 -17.00 150.00   52
 29  \w    150.00 175.00   0.50    4.73    --   94.70  33.00 150.00   50
 30  \w     27.00  52.00   0.50    4.73    --   94.70 -17.00 150.00   50
 31  \w     85.00 110.00   0.50    4.73    --   94.70  33.00 150.00   50
 32  \w     42.00 116.00   0.50    4.73    --   94.70 -33.00-150.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Pro II AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0294024000
_diffrn_orient_matrix_UB_12      0.0278446000
_diffrn_orient_matrix_UB_13      -0.0582510000
_diffrn_orient_matrix_UB_21      0.0483447000
_diffrn_orient_matrix_UB_22      -0.0475675000
_diffrn_orient_matrix_UB_23      -0.0189664000
_diffrn_orient_matrix_UB_31      -0.0683743000
_diffrn_orient_matrix_UB_32      -0.0456453000
_diffrn_orient_matrix_UB_33      -0.0157613000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            52056
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        62.993
_diffrn_reflns_theta_max         62.993
_diffrn_reflns_theta_min         2.544
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.786
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       prism
_exptl_crystal_F_000             3976
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.493
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         15168
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0968
_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^)+(0.1895P)^2^+7.6376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2632
_refine_ls_wR_factor_ref         0.2798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11556
_reflns_number_total             15168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02406c2.cif
_cod_data_source_block           2022-9-5-a6-3_auto_sq_sq
_cod_database_code               7711465
_chemical_oxdiff_formula         'Zn C H O N'
_chemical_oxdiff_usercomment     'Zn C H O N'
_diffrn_oxdiff_digest_frames
;
018c0e10d13f98e689cd9f6b60ffdf7a1e000283e8f
;
_diffrn_oxdiff_digest_hkl
;
01ece8368d92cb8c3078cf17cf8be0ff20928d
;
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C48-N5
 1.45 with sigma of 0.01
 N5-C49
 1.45 with sigma of 0.01
 N5-C50
 1.45 with sigma of 0.01
 C50-C49
 2.51 with sigma of 0.01
 H20B-O20
 0.85 with sigma of 0.01
 O20-H20A
 0.85 with sigma of 0.01
 O21-H21B
 0.85 with sigma of 0.01
 O21-H21A
 0.85 with sigma of 0.01
 H20B-H20A
 1.39 with sigma of 0.01
 H21A-H21B
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C50 \\sim C48 \\sim O17 \\sim N5 \\sim C49: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C46) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4.a Riding coordinates:
 N1(H1), O20(H20A), O20(H20B), O21(H21A), O21(H21B)
4.b Rotating group:
 O19(H19A,H19B)
4.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C7(H7), C17(H17), C18(H18), C29(H29), C4(H4), C21(H21), C22(H22),
 C10(H10), N4(H4A), C26(H26), C13(H13), C9(H9), N3(H3), C42(H42), C14(H14),
 C35(H35), C36(H36), C40(H40), C43(H43), C33(H33), C32(H32), C39(H39), C45(H45),
  C48(H48)
4.d Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C46(H46A,H46B,H46C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C)
;
_shelx_fab_checksum              56016
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.347
_oxdiff_exptl_absorpt_empirical_full_min 0.537
_platon_squeeze_void_probe_radius 1.20