A metal complex based fluorescent chemodosimeter for selective detection of 2,4-dinitrophenol and picric acid in aqueous media
Pramanik, Abhishek; Majumder, Samit; Sparkes, Hazel A.; Mohanta, Sasankasekhar; Dalton Transactions  (2022) –; doi:10.1039/D2DT01808J

data_7711244
_publ_section_title
;
 A metal complex based fluorescent chemodosimeter for selective detection
 of 2,4-dinitrophenol and picric acid in aqueous media
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01808J
_journal_year                    2022
_chemical_formula_moiety         'C16 H25 N13 O Zn2'
_chemical_formula_sum            'C16 H25 N13 O Zn2'
_chemical_formula_weight         546.23
_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             2019-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-15 deposited with the CCDC.	2022-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.723(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3387(7)
_cell_length_b                   10.7536(6)
_cell_length_c                   14.2438(8)
_cell_measurement_reflns_used    9423
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.37
_cell_volume                     2196.1(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_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      100(2)
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker Apex II kappa CCDC area detector'
_diffrn_measurement_device_type  'Bruker Apex II kappa CCDC area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29945
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.420
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.223
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1277 before and 0.0742 after correction. The Ratio of minimum to maximum transmission is 0.6723. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.467
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.224
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4022
_refine_ls_number_restraints     191
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0158P)^2^+17.2997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1262
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3396
_reflns_number_total             4022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01808j3.cif
_cod_data_source_block           1
_cod_database_code               7711244
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.636
_shelx_estimated_absorpt_t_min   0.423
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7-C11A \\sim C7-C11
 with sigma of 0.01
 C12-C11 \\sim C12A-C11A
 with sigma of 0.01
 Zn1-N8A \\sim Zn1-N8
 with sigma of 0.01
 Zn2-N8A \\sim Zn2-N8
 with sigma of 0.01
 N12A-N13A \\sim N13-N12 \\sim N10-N9 \\sim N9A-N10A \\sim N7-N6
 with sigma of 0.01
 N12-N11 \\sim N12A-N11 \\sim N9-N8 \\sim N8A-N9A \\sim N5-N6
 with sigma of 0.01
3. Restrained planarity
 C5, C9, C10, C11A
 with sigma of 0.01
 C5, C9, C10, C6, C7, C8, C11
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C5 \\sim C9 \\sim C10 \\sim C6 \\sim C7 \\sim C8 \\sim C11 \\sim C12: within 2A
with sigma of 0.003 and sigma for terminal atoms of 0.006
N8 \\sim N9 \\sim N10 \\sim N8A \\sim N9A \\sim N10A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
N11 \\sim N12 \\sim N13 \\sim N12A \\sim N13A: within 2A with sigma of 0.003
and sigma for terminal atoms of 0.006
Uanis(C11A) = Uanis(C11)
5. Others
 Sof(N8A)=Sof(N9A)=Sof(N10A)=1-FVAR(1)
 Sof(N8)=Sof(N9)=Sof(N10)=FVAR(1)
 Sof(N12A)=Sof(N13A)=1-FVAR(2)
 Sof(N12)=Sof(N13)=FVAR(2)
 Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(3)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 N1(H1), N4(H4)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C14(H14A,H14B), C15(H15A,H15B), C11(H11A,H11B),
 C11A(H11C,H11D)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4A), C13(H13), C6(H6), C8(H8)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C12A(H12D,H12E,H12F)
;
_shelx_res_checksum              81136
_shelx_hkl_checksum              62941
_olex2_submission_special_instructions 'No special instructions were received'