Selective sensing of picric acid using a Zn(II)-metallacycle: experimental and theoretical validation of the sensing mechanism and quantitative analysis of sensitivity in contact mode detection.
Jaswal, Vishakha; Pachisia, Sanya; Chaudhary, Jagrity; Rangan, Krishnan; Sarkar, Madhushree; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14710–14724; doi:10.1039/d4dt01771d

data_7716818
_publ_section_title
;
 Selective sensing of picric acid using a Zn(II)-metallacycle:
 experimental and theoretical validation of the sensing mechanism and
 quantitative analysis of sensitivity in contact mode detection.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14710
_journal_page_last               14724
_journal_paper_doi               10.1039/d4dt01771d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C76 H52 Cl4 N12 O14 Zn2, 4(C3 H7 N O)'
_chemical_formula_sum            'C88 H80 Cl4 N16 O18 Zn2'
_chemical_formula_weight         1922.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-20 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.188(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.2400(3)
_cell_length_b                   11.9521(2)
_cell_length_c                   21.5421(4)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      78.6660
_cell_measurement_theta_min      4.1310
_cell_volume                     4393.59(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.962
_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    -85.00 -55.00   0.50   10.00    --    0.00 -37.00-150.00   60
  2  \w    -65.00  14.00   0.50   10.00    --    0.00 -37.00 -90.00  158
  3  \w     -8.00  18.00   0.50   10.00    --    0.00 -37.00-150.00   52
  4  \w    -89.00 -50.00   0.50   10.00    --    0.00 -37.00-180.00   78
  5  \w    -23.00  28.00   0.50   10.00    --    0.00 -77.00-150.00  102
  6  \w    108.00 134.00   0.50   40.00    --  107.20 -77.00  90.00   52
  7  \w     18.00  58.00   0.50   40.00    --  107.20 -77.00  90.00   80
  8  \w     18.00 132.00   0.50   40.00    --  107.20 -61.00-150.00  228
  9  \w     54.00 106.00   0.50   40.00    --  107.20 -82.00 150.00  104
 10  \w    169.00 196.00   0.50   40.00    --  107.20  61.00 120.00   54
 11  \w     18.00 126.00   0.50   40.00    --  107.20 -30.00   0.00  216
 12  \w    100.00 144.00   0.50   40.00    --  107.20  61.00 120.00   88
 13  \w     34.00 134.00   0.50   40.00    --  107.20 -77.00-150.00  200
 14  \w    151.00 180.00   0.50   40.00    --  107.20  30.00-120.00   58
 15  \w     18.00 148.00   0.50   40.00    --  107.20   0.00-120.00  260
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB 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      -0.0870654000
_diffrn_orient_matrix_UB_12      -0.0198621000
_diffrn_orient_matrix_UB_13      0.0053864000
_diffrn_orient_matrix_UB_21      0.0210312000
_diffrn_orient_matrix_UB_22      -0.0144948000
_diffrn_orient_matrix_UB_23      0.0714750000
_diffrn_orient_matrix_UB_31      -0.0112828000
_diffrn_orient_matrix_UB_32      0.1265491000
_diffrn_orient_matrix_UB_33      0.0090363000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15886
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.676
_diffrn_reflns_theta_min         4.147
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.446
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         11452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0614
_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^)+(0.1061P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11452
_reflns_number_total             11452
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9997\% 
around [0.51 -0.00 0.86] (reciprocal) or [0.71 0.00 0.71] (direct)
;
_cod_data_source_file            d4dt01771d2.cif
_cod_data_source_block           exp921_twinmodel_20211208_twin1_hklf4
_cod_depositor_comments          'Adding full bibliography for 7716818.cif.'
_cod_database_code               7716818
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C44 H40 Cl2 N8 O9 Zn'
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.681
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7433(8)
 0.2567(8)
2. 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
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), C2(H2A), C4(H4), C6(H6), C10(H10), C12(H12), C13(H13),
  C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
 C23(H23), C24(H24), C27(H27), C28(H28), C30(H30), C31(H31), C34(H34), C35(H35),
  C37(H37), C38(H38), C39(H39), C42(H42)
3.b Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C)
;
_shelx_res_checksum              28733
_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 1.647
_oxdiff_exptl_absorpt_empirical_full_min 0.710
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2