New Ln-MOFs based on mixed organic ligands: synthesis, structure and efficient luminescence sensing of the Hg2+ ion in aqueous solutions
Wang, Shu-ju; Li, Qian; Xiu, Guan-Lin; You, Li-Xin; Ding, Fu; Van Deun, Rik; Dragutan, Ileana; Dragutan, Valerian; Sun, Yaguang; Dalton Transactions  (2021) –; doi:10.1039/D1DT02687A

data_7708513
_publ_section_title
;
 New Ln-MOFs based on mixed organic ligands: synthesis, structure and
 efficient luminescence sensing of the Hg2+ ion in aqueous solutions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02687A
_journal_year                    2021
_chemical_formula_moiety
'C144 H106 N8 O25 S6 Tb4, H2 O, C12 H8 N2, H2 O0.63, H2 O0.6, 0.77(O1)'
_chemical_formula_sum            'C156 H120 N10 O28 S6 Tb4'
_chemical_formula_weight         3410.65
_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
_audit_creation_date             2019-01-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-09 deposited with the CCDC.	2021-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                108.9390(10)
_cell_angle_beta                 90.4640(10)
_cell_angle_gamma                98.1850(10)
_cell_formula_units_Z            2
_cell_length_a                   11.47990(10)
_cell_length_b                   22.0925(2)
_cell_length_c                   29.0010(3)
_cell_measurement_reflns_used    57054
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      74.2060
_cell_measurement_theta_min      3.8710
_cell_volume                     6874.59(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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      N~2~
_diffrn_ambient_temperature      100.00(13)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9963
_diffrn_measured_fraction_theta_max 0.9757
_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    -30.00  89.00   0.50    2.61    --    0.00  57.00  90.00  238
  2  \w    -35.00  89.00   0.50    2.61    --    0.00  77.00  90.00  248
  3  \w    -89.00  32.00   0.50    2.61    --    0.00 -38.00  90.00  242
  4  \w    -89.00  30.00   0.50    2.61    --    0.00 -57.00  30.00  238
  5  \w    -35.00  89.00   0.50    2.61    --    0.00  77.00-120.00  248
  6  \w     62.00 185.00   0.50   11.00    --   95.80  37.00 111.94  246
  7  \w      6.00 133.00   0.50   11.00    --   95.80 -82.00-180.00  254
  8  \w     58.00 185.00   0.50   11.00    --   95.80  82.00 -30.00  254
  9  \w      6.00 133.00   0.50   11.00    --   95.80 -82.00 -60.00  254
 10  \w      6.00 126.00   0.50   11.00    --   95.80 -61.00  30.00  240
 11  \w      6.00 126.00   0.50   11.00    --   95.80 -61.00-120.00  240
 12  \w     65.00 185.00   0.50   11.00    --   95.80  45.00-180.00  240
 13  \w      6.00 133.00   0.50   11.00    --   95.80 -82.00 -30.00  254
 14  \w      6.00 133.00   0.50   11.00    --   95.80 -82.00 120.00  254
 15  \w      6.00 133.00   0.50   11.00    --   95.80 -82.00-120.00  254
 16  \w     65.00 185.00   0.50   11.00    --   95.80  45.00-150.00  240
 17  \w      6.00 133.00   0.50   11.00    --   95.80 -82.00 -90.00  254
 18  \w     66.00 185.00   0.50   11.00    --   95.80  49.00 132.93  238
 19  \w      6.00 133.00   0.50   11.00    --   95.80 -82.00  30.00  254
 20  \w      6.00 128.00   0.50   11.00    --   95.80 -82.00  60.00  244
 21  \w    108.00 185.00   0.50   11.00    --   95.80  40.00  75.47  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0029113000
_diffrn_orient_matrix_UB_12      0.0677384000
_diffrn_orient_matrix_UB_13      -0.0037797000
_diffrn_orient_matrix_UB_21      0.0097992000
_diffrn_orient_matrix_UB_22      0.0293384000
_diffrn_orient_matrix_UB_23      0.0561220000
_diffrn_orient_matrix_UB_31      0.1354202000
_diffrn_orient_matrix_UB_32      0.0108024000
_diffrn_orient_matrix_UB_33      -0.0008704000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            131914
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.547
_diffrn_reflns_theta_min         3.075
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    11.432
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       block
_exptl_crystal_F_000             3412
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.649
_refine_diff_density_min         -1.728
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1908
_refine_ls_number_reflns         27405
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0716P)^2^+6.7338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1285
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23081
_reflns_number_total             27405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02687a2.cif
_cod_data_source_block           wsj-2
_cod_original_cell_volume        6874.58(12)
_cod_database_code               7708513
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C84A-S5A \\sim C84-S5
 with sigma of 0.01
 C84A-C81 \\sim C81-C84
 with sigma of 0.01
 C84-C82 \\sim C82-C84A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S5 \\sim C85 \\sim C84 \\sim C84A \\sim S5A \\sim C85A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Sof(H68c)=Sof(H68d)=Sof(H69c)=Sof(H69d)=Sof(S05Q)=1-FVAR(1)
 Sof(S3A)=Sof(H68a)=Sof(H68b)=Sof(H69a)=Sof(H69b)=FVAR(1)
 Sof(C84A)=Sof(H84c)=Sof(H84d)=Sof(S5A)=Sof(C85A)=Sof(H85c)=Sof(H85d)=1-FVAR(2)
 Sof(S5)=Sof(C85)=Sof(H85a)=Sof(H85b)=Sof(C84)=Sof(H84a)=Sof(H84b)=FVAR(2)
 Fixed Sof: S2A(0.5) S2(0.5) H36c(0.5) H36d(0.5) H36a(0.5) H36b(0.5) H37c(0.5)
 H37d(0.5) H37a(0.5) H37b(0.5)
5.a Rotating group:
 O11(H11a,H11b)
5.b Secondary CH2 refined with riding coordinates:
 C101(H10a,H10b), C100(H10c,H10d), C20(H20a,H20b), C21(H21a,H21b), C53(H53a,
 H53b), C52(H52a,H52b), C68(H68a,H68b), C68(H68c,H68d), C85(H85a,H85b),
 C36(H36c,H36d), C36(H36a,H36b), C69(H69a,H69b), C69(H69c,H69d), C37(H37c,H37d),
  C37(H37a,H37b), C84(H84a,H84b), C84A(H84c,H84d), C85A(H85c,H85d)
5.c Aromatic/amide H refined with riding coordinates:
 C58(H58), C104(H104), C51(H51), C31(H31), C109(H109), C95(H95), C106(H106),
 C56(H56), C119(H119), C72(H72), C63(H63), C96(H96), C118(H118), C15(H15),
 C98(H98), C50(H50), C145(H145), C27(H27), C16(H16), C154(H154), C155(H155),
 C99(H99), C107(H107), C35(H35), C111(H111), C59(H59), C117(H117), C110(H110),
 C146(H146), C67(H67), C26(H26), C103(H103), C147(H147), C121(H121), C131(H131),
  C153(H153), C24(H24), C47(H47), C48(H48), C129(H129), C43(H43), C79(H79),
 C40(H40), C18(H18), C19(H19), C55(H55), C66(H66), C151(H151), C150(H150),
 C71(H71), C83(H83), C10(H10), C23(H23), C130(H130), C127(H127), C8(H8),
 C74(H74), C114(H114), C1(H1), C32(H32), C42(H42), C12(H12), C122(H122), C2(H2),
  C88(H88), C64(H64), C80(H80), C123(H123), C82(H82), C115(H115), C90(H90),
 C3(H3), C34(H34), C9(H9), C126(H126), C75(H75), C11(H11), C91(H91), C87(H87),
 C39(H39)
;
_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 1.682
_oxdiff_exptl_absorpt_empirical_full_min 0.717