The synthesis, structural elucidation and fluorescent sensitization detection to Hg2+ based on two lanthanide-organic complexes
Li, Rong-fang; Zhang, Ya-wen; Liu, Xin-fang; Chang, Xin-hong; Feng, Xun; Inorganica Chimica Acta 502 (2020) 119370–; doi:10.1016/j.ica.2019.119370

data_1565413
_publ_section_title
;
 The synthesis, structural elucidation and fluorescent sensitization
 detection to Hg2+ based on two lanthanide-organic complexes
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119370
_journal_paper_doi               10.1016/j.ica.2019.119370
_journal_volume                  502
_journal_year                    2020
_chemical_formula_moiety         'C36 H24 Dy2 N6 O15, H2 O'
_chemical_formula_sum            'C36 H27 Dy2 N6 O16'
_chemical_formula_weight         1124.63
_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   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                94.986(2)
_cell_angle_beta                 103.496(2)
_cell_angle_gamma                101.309(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3536(3)
_cell_length_b                   12.1823(3)
_cell_length_c                   14.2259(4)
_cell_measurement_reflns_used    12218
_cell_measurement_temperature    290.8(3)
_cell_measurement_theta_max      28.9770
_cell_measurement_theta_min      3.7760
_cell_volume                     1857.89(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      290.8(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.878
_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   3.00   1.00    3.92    --  -15.84 -38.00-150.00   88
  2  \w    -68.00   1.00   1.00    3.92    --  -15.84 122.00  80.36   69
  3  \w    -10.00  84.00   1.00    3.92    --   16.93  77.00 -30.00   94
  4  \w     44.00  76.00   1.00    3.92    --   16.93-134.00 -58.00   32
  5  \w    -20.00  56.00   1.00    3.92    --   16.93 -99.00  30.00   76
  6  \w    -48.00  30.00   1.00    3.92    --   16.93 -77.00-150.00   78
  7  \w      7.00  84.00   1.00    3.92    --   16.93  57.00  90.00   77
  8  \w    -49.00  34.00   1.00    3.92    --   16.93 -38.00 -90.00   83
  9  \w     -9.00  84.00   1.00    3.92    --   16.93  77.00-180.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0090612000
_diffrn_orient_matrix_UB_12      0.0144921000
_diffrn_orient_matrix_UB_13      0.0467708000
_diffrn_orient_matrix_UB_21      -0.0581349000
_diffrn_orient_matrix_UB_22      0.0116857000
_diffrn_orient_matrix_UB_23      -0.0222158000
_diffrn_orient_matrix_UB_31      -0.0297121000
_diffrn_orient_matrix_UB_32      -0.0569970000
_diffrn_orient_matrix_UB_33      -0.0002421000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.878
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29028
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.312
_diffrn_reflns_theta_min         3.444
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.076
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_description       block
_exptl_crystal_F_000             1090
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.207
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         8937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+0.3376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7394
_reflns_number_total             8937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Dy-2.cif
_cod_data_source_block           lrf-p4-dy
_cod_database_code               1565413
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O16(H16a,H16b)
2.b Rotating group:
 O3(H3a,H3b), O14(H14a,H14b), O15(H15a,H15b)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11), C15(H15), C17(H17),
 C18(H18), C21(H21), C23(H23), C24(H24), C26(H26), C28(H28), C29(H29), C32(H32),
  C34(H34), C35(H35)
;
_shelx_res_checksum              30800
_shelx_hkl_checksum              27024
_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 2.117
_oxdiff_exptl_absorpt_empirical_full_min 0.294