Visual detection of Hg2+ without interference by alkali and alkaline earth metal ions using an iron(iii) complex in a hetero-bimetallic environment
Paik, Somnath; Ray, Manabendra; New Journal of Chemistry 49 (2025) 9980–9989; doi:10.1039/D5NJ00233H

data_7063822
_publ_section_title
;
 Visual detection of Hg2+ without interference by alkali and alkaline
 earth metal ions using an iron(iii) complex in a hetero-bimetallic
 environment
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9980
_journal_page_last               9989
_journal_paper_doi               10.1039/D5NJ00233H
_journal_volume                  49
_journal_year                    2025
_chemical_absolute_configuration syn
_chemical_compound_source        'Laboratory Synthesized'
_chemical_formula_moiety         '(C76 H72 Ca Fe2 N8 O16), 2.5(C3 H7 N O), 4(O)'
_chemical_formula_sum            'C83.5 H89.5 Ca Fe2 N10.5 O22.5'
_chemical_formula_weight         1751.93
_chemical_name_common            CalciumComplex
_chemical_name_systematic        'Inorganic Complex'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2m3q3l
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-05-06 deposited with the CCDC.	2025-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.065(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.397(3)
_cell_length_b                   14.023(4)
_cell_length_c                   25.188(6)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.22
_cell_volume                     4659(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'CSD Mercury'
_computing_publication_material  'CSD Encifer'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Quest CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            64959
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        19.995
_diffrn_reflns_theta_max         19.995
_diffrn_reflns_theta_min         1.871
_diffrn_source                   'fine focus 1.75 kW sealed tube'
_diffrn_source_type              'Bruker Smart Apex CCD'
_exptl_absorpt_coefficient_mu    0.439
_exptl_absorpt_correction_T_max  0.7344
_exptl_absorpt_correction_T_min  0.6539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       Block
_exptl_crystal_F_000             1832
_exptl_crystal_recrystallization_method
'Slow evaporation of complex solution in MeOH-DMF mixed solvent'
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 2778 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.064(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.320
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         8677
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.318
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=exp[3.0000(sin\q/\l)^2^)]/[\s^2^(Fo^2^)+
(0.0894P)^2^+4.0411P+0.0400] where P=(0.1000Fo^2^+0.9000Fc^2^)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1668
_reflns_Friedel_coverage         0.895
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7039
_reflns_number_total             8689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj00233h2.cif
_cod_data_source_block           Calcium_Structure_Complex_4
_cod_depositor_comments
'Adding full bibliography for 7063821--7063824.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C83.50 H89.50 Ca Fe2 N10.50 O22.50'
_cod_database_code               7063822
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.945
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              9303
_shelx_fab_checksum              1844