Development of a novel carboxamide-based off‒on switch fluorescence sensor: Hg2+, Zn2+ and Cd2+
Kiani, Mahsa; Bagherzadeh, Mojtaba; Meghdadi, Soraia; Rabiee, Navid; Abbasi, Alireza; Schenk-Joß, Kurt; Tahriri, Mohammadreza; Tayebi, Lobat; Webster, Thomas J.; New Journal of Chemistry 44 (2020) 11841–11852; doi:10.1039/D0NJ02595J

data_7059759
_publ_section_title
;
 Development of a novel carboxamide-based off--on switch fluorescence
 sensor: Hg2+, Zn2+ and Cd2+
;
_journal_issue                   27
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11841
_journal_page_last               11852
_journal_paper_doi               10.1039/D0NJ02595J
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety
'C18 H16 N6 O4 S2 Zn, 0.12(C H2 Cl2), 0.81(C2 H6 O)'
_chemical_formula_sum            'C19.74 H21.1 Cl0.24 N6 O4.81 S2 Zn'
_chemical_formula_weight         557.36
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-11-30
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.11 svn.r3662 for OlexSys, GUI svn.r5962)
;
_audit_update_record
;
2019-11-30 deposited with the CCDC.	2020-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.38(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.070(3)
_cell_length_b                   11.350(2)
_cell_length_c                   14.666(3)
_cell_measurement_temperature    100.0
_cell_volume                     2340.1(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6957
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4111
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.559
_diffrn_reflns_theta_max         24.559
_diffrn_reflns_theta_min         2.222
_exptl_absorpt_coefficient_mu    1.230
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       prism
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.119
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         4111
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+10.5454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1924
_refine_ls_wR_factor_ref         0.1925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4029
_reflns_number_total             4111
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02595j1.cif
_cod_data_source_block           sm2
_cod_depositor_comments
;Adding full bibliography for 7059758--7059759.cif.

 Adding full bibliography for 7059758--7059759.cif.
;
_cod_original_cell_volume        2340.2(8)
_cod_original_formula_sum        'C19.74 H21.10 Cl0.24 N6 O4.81 S2 Zn'
_cod_database_code               7059759
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.589(4)
 0.411(4)
2. 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, All O(H) groups, All O(H,H) groups
3. Restrained distances
 O5-C21
 2.366 with sigma of 0.04
 Cl2-C19
 1.765 with sigma of 0.02
 Cl1-Cl2
 2.916 with sigma of 0.04
 C20-C21
 1.51 with sigma of 0.02
 Cl1-C19
 1.777 with sigma of 0.02
 O5-C20
 1.425 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim C19: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
5. Others
 Fixed Sof: Cl1(0.12) Cl2(0.12) C19(0.12) H19A(0.12) H19B(0.12) O5(0.81)
 H5(0.81) C20(0.81) H20A(0.81) H20B(0.81) C21(0.81) H21A(0.81) H21B(0.81)
 H21C(0.81)
6.a Rotating group:
 O3(H3A,H3B), O4(H4A,H4B)
6.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C15(H15),
 C16(H16), C17(H17), C18(H18)
6.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C)
6.e Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_shelx_res_checksum              9889
_olex2_submission_special_instructions 'No special instructions were received'