A highly selective pyridoxal-based chemosensor for the detection of Zn(ii) and application in live-cell imaging; X-ray crystallography of pyridoxal-TRIS Schiff-base Zn(ii) and Cu(ii) complexes
Hussain, Anwar; Mariappan, Kadarkaraisamy; Cork, Dawson C.; Lewandowski, Luke D.; Shrestha, Prem K.; Giri, Samiksha; Wang, Xuejun; Sykes, Andrew G.; RSC Advances 11 (2021) 34181–34192; doi:10.1039/D1RA05763D

data_7243796
_publ_section_title
;
 A highly selective pyridoxal-based chemosensor for the detection of
 Zn(ii) and application in live-cell imaging; X-ray crystallography of
 pyridoxal-TRIS Schiff-base Zn(ii) and Cu(ii) complexes
;
_journal_issue                   54
_journal_name_full               'RSC Advances'
_journal_page_first              34181
_journal_page_last               34192
_journal_paper_doi               10.1039/D1RA05763D
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C24 H34 N4 O10 Zn, 5(H2 O)'
_chemical_formula_sum            'C24 H44 N4 O15 Zn'
_chemical_formula_weight         694.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-07-08 deposited with the CCDC.	2021-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3659(17)
_cell_length_b                   8.7855(9)
_cell_length_c                   16.9217(19)
_cell_measurement_reflns_used    23510
_cell_measurement_temperature    106(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      2.0
_cell_volume                     3027.7(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      106(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1272
_diffrn_reflns_av_unetI/netI     0.1097
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23510
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.359
_diffrn_reflns_theta_min         2.000
_exptl_absorpt_coefficient_mu    0.889
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rectangle
_exptl_crystal_F_000             1464
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol, Diethylether, Water'
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Flack x determined using 1246 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         5476
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.091
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0631P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1505
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                3725
_reflns_number_total             5476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra05763d2.cif
_cod_data_source_block           shelx_CCDC1
_cod_database_code               7243796
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.940
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              70056