A new dioxo-molybdenum complex derived from an amide-based imine derivative for the fluorescence recognition of Zr(iv) with phosphatase activity
De, Amit Kumar; Shaym, Tandrim; Ghosh, Subhasis; Dogra, Sunanda; Roy Choudhury, Angshuman; Das, Debasis; RSC Advances 16 (2026) 11130–11136; doi:10.1039/D5RA04804D

data_7251683
_publ_section_title
;
 A new dioxo-molybdenum complex derived from an amide-based imine
 derivative for the fluorescence recognition of Zr(iv) with phosphatase
 activity
;
_journal_issue                   12
_journal_name_full               'RSC Advances'
_journal_page_first              11130
_journal_page_last               11136
_journal_paper_doi               10.1039/D5RA04804D
_journal_volume                  16
_journal_year                    2026
_chemical_formula_moiety         'C17 H17 Mo N3 O7, C3 H7 N O'
_chemical_formula_sum            'C20 H24 Mo N4 O8'
_chemical_formula_weight         544.37
_chemical_name_systematic        DDAD-13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-17
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-05-06 deposited with the CCDC.	2026-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                104.639(3)
_cell_angle_beta                 93.972(2)
_cell_angle_gamma                101.116(3)
_cell_formula_units_Z            2
_cell_length_a                   6.5396(2)
_cell_length_b                   12.7039(5)
_cell_length_c                   14.4697(4)
_cell_measurement_reflns_used    7588
_cell_measurement_temperature    200.00(1)
_cell_measurement_theta_max      24.9640
_cell_measurement_theta_min      2.9000
_cell_volume                     1132.43(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(1)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -69.00 118.20   0.30    4.00    --   29.89  54.00-120.00  624
  2  \w    -69.00 118.20   0.30    4.00    --   29.89  54.00 -30.00  624
  3  \w    -69.00 118.20   0.30    4.00    --   29.89  54.00 -30.00  624
  4  \w    -66.00 116.10   0.30    4.00    --   29.89  54.00 120.00  607
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0891584000
_diffrn_orient_matrix_UB_12      0.0197550000
_diffrn_orient_matrix_UB_13      0.0161337000
_diffrn_orient_matrix_UB_21      -0.0384190000
_diffrn_orient_matrix_UB_22      -0.0041744000
_diffrn_orient_matrix_UB_23      -0.0481407000
_diffrn_orient_matrix_UB_31      -0.0546319000
_diffrn_orient_matrix_UB_32      -0.0555724000
_diffrn_orient_matrix_UB_33      -0.0054152000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13646
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.933
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       plate
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.382
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0280P)^2^+2.0201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0853
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3721
_reflns_number_total             4004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra04804d2.cif
_cod_data_source_block           ddad-13
_cod_database_code               7251683
_shelx_shelxl_version_number     2018/3
_cell_oxdiff_angle_alpha         104.639(3)
_cell_oxdiff_angle_beta          93.972(2)
_cell_oxdiff_angle_gamma         101.116(3)
_cell_oxdiff_length_a            6.5396(2)
_cell_oxdiff_length_b            12.7039(5)
_cell_oxdiff_length_c            14.4697(4)
_cell_oxdiff_measurement_reflns_used 7588
_cell_oxdiff_volume              1132.43(6)
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.987
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C15(H15), C3(H3), C6(H6), C14(H14), C4(H4), C11(H11), C18(H18),
 C13(H13), C12(H12)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C20(H20A,H20B,
 H20C)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O1(H1)
;
_shelx_res_checksum              25099
_olex2_submission_original_sample_id DDAD-13
_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 1.228
_oxdiff_exptl_absorpt_empirical_full_min 0.834