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_1565414
_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 N6 O15 Tb2, H2 O'
_chemical_formula_sum            'C36 H26 N6 O16 Tb2'
_chemical_formula_weight         1116.47
_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     iterative
_cell_angle_alpha                95.074(3)
_cell_angle_beta                 103.481(3)
_cell_angle_gamma                101.049(3)
_cell_formula_units_Z            2
_cell_length_a                   11.3664(4)
_cell_length_b                   12.1986(4)
_cell_length_c                   14.2543(5)
_cell_measurement_reflns_used    15110
_cell_measurement_temperature    293.2(3)
_cell_measurement_theta_max      28.9200
_cell_measurement_theta_min      3.5290
_cell_volume                     1867.90(12)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.2(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 0.875
_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    -82.00   4.00   1.00    2.64    --  -15.84 -77.00  90.00   86
  2  \w    -13.00  50.00   1.00    2.64    --  -15.84  77.00-150.00   63
  3  \w    -81.00   9.00   1.00    2.64    --  -15.84 -77.00-150.00   90
  4  \w    -68.00 -36.00   1.00    2.64    --  -15.84 122.00  -2.19   32
  5  \w    -39.00 -13.00   1.00    2.64    --  -15.84  77.00 -30.00   26
  6  \w    -10.00  50.00   1.00    2.64    --  -15.84  77.00 -30.00   60
  7  \w    -54.00  -7.00   1.00    2.64    --  -15.84 -57.00 -30.00   47
  8  \w    -40.00  24.00   1.00    2.64    --   16.93 -57.00  60.00   64
  9  \w      0.00  81.00   1.00    2.64    --   16.93  38.00   0.00   81
 10  \w    -13.00  56.00   1.00    2.64    --   16.93 -99.00 -60.00   69
 11  \w    -18.00  56.00   1.00    2.64    --   16.93 -99.00-180.00   74
;
_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      0.0355805000
_diffrn_orient_matrix_UB_12      -0.0135956000
_diffrn_orient_matrix_UB_13      -0.0323677000
_diffrn_orient_matrix_UB_21      0.0542978000
_diffrn_orient_matrix_UB_22      0.0339937000
_diffrn_orient_matrix_UB_23      0.0326272000
_diffrn_orient_matrix_UB_31      0.0105600000
_diffrn_orient_matrix_UB_32      -0.0473195000
_diffrn_orient_matrix_UB_33      0.0236255000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.875
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29241
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.293
_diffrn_reflns_theta_min         3.437
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.840
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79119
_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 brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_description       block
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_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      1.028
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+1.8101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0582
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7801
_reflns_number_total             8937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Tb-1.cif
_cod_data_source_block           lrf-p4-tb
_cod_database_code               1565414
_shelx_estimated_absorpt_t_max   0.597
_shelx_estimated_absorpt_t_min   0.485
_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), O9(H9A,H9B), O10(H10A,H10B)
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), C20(H20), C22(H22), C23(H23), C26(H26), C28(H28), C29(H29), C33(H33),
  C35(H35), C36(H36)
;
_shelx_res_checksum              93024
_shelx_hkl_checksum              71858
_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 1.407
_oxdiff_exptl_absorpt_empirical_full_min 0.786