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_7708512
_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 Eu4 N8 O25 S6, 3(H2 O), C12 H8 N2'
_chemical_formula_sum            'C156 H120 Eu4 N10 O28 S6'
_chemical_formula_weight         3382.81
_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
_audit_creation_date             2021-08-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-11 deposited with the CCDC.	2021-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                108.9420(10)
_cell_angle_beta                 90.1040(10)
_cell_angle_gamma                98.5400(10)
_cell_formula_units_Z            2
_cell_length_a                   11.49550(10)
_cell_length_b                   22.0977(3)
_cell_length_c                   29.0980(3)
_cell_measurement_reflns_used    42210
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.0510
_cell_measurement_theta_min      3.9250
_cell_volume                     6903.91(14)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.963
_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     56.00  89.00   0.50    0.80    --    0.00  57.00  30.00   66
  2  \w     20.00  78.00   0.50    0.80    --    0.00  57.00 120.00  116
  3  \w    -88.00 -17.00   0.50    0.80    --    0.00 -38.00 150.00  142
  4  \w    -52.00  18.00   0.50    0.80    --    0.00 -38.00-120.00  140
  5  \w      8.00  33.00   0.50    0.80    --    0.00 -82.00 120.00   50
  6  \w    -89.00 -35.00   0.50    0.80    --    0.00 -82.00 120.00  108
  7  \w    -21.00  22.00   0.50    0.80    --    0.00  57.00  30.00   86
  8  \w    137.00 163.00   0.50    4.50    --   95.80  82.00 -90.00   52
  9  \w     78.00 104.00   0.50    4.50    --   95.80  82.00 -90.00   52
 10  \w     83.00 131.00   0.50    4.50    --   95.80 -82.00-150.00   96
 11  \w     92.00 125.00   0.50    4.50    --   95.80 -30.00-150.00   66
 12  \w     65.00 105.00   0.50    4.50    --   95.80  61.00-180.00   80
 13  \w    116.00 142.00   0.50    4.50    --   95.80  61.00-180.00   52
 14  \w     58.00 104.00   0.50    4.50    --   95.80 -82.00 -90.00   92
 15  \w      6.00  84.00   0.50    4.50    --   95.80 -30.00-150.00  156
 16  \w      7.00 133.00   0.50    4.50    --   95.80 -82.00   0.00  252
 17  \w     88.00 126.00   0.50    4.50    --   95.80 -45.00 150.00   76
 18  \w     21.00  65.00   0.50    4.50    --   95.80 -45.00 150.00   88
 19  \w     63.00 179.00   0.50    4.50    --   95.80  30.00  90.00  232
 20  \w     51.00 119.00   0.50    4.50    --   95.80 -82.00-180.00  136
 21  \w     56.00 105.00   0.50    4.50    --   95.80 -82.00  90.00   98
 22  \w      6.00  45.00   0.50    4.50    --   95.80 -82.00-180.00   78
 23  \w     43.00  77.00   0.50    4.50    --   95.80 -82.00 120.00   68
 24  \w     94.00 132.00   0.50    4.50    --   95.80 -82.00 120.00   76
 25  \w     16.00  41.00   0.50    4.50    --   95.80 -82.00 -30.00   50
 26  \w     79.00 105.00   0.50    4.50    --   95.80 -82.00 -30.00   52
 27  \w      9.00 108.00   0.50    4.50    --   95.80 -61.00   0.00  198
 28  \w      6.00  73.00   0.50    4.50    --   95.80 -82.00-150.00  134
 29  \w    111.00 149.00   0.50    4.50    --   95.80  61.00  30.00   76
 30  \w     81.00 180.00   0.50    4.50    --   95.80  30.00 120.00  198
;
_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      0.0053483000
_diffrn_orient_matrix_UB_12      0.0325700000
_diffrn_orient_matrix_UB_13      0.0556343000
_diffrn_orient_matrix_UB_21      0.0454666000
_diffrn_orient_matrix_UB_22      0.0660014000
_diffrn_orient_matrix_UB_23      -0.0060834000
_diffrn_orient_matrix_UB_31      -0.1277555000
_diffrn_orient_matrix_UB_32      0.0123634000
_diffrn_orient_matrix_UB_33      -0.0030004000
_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  0.0458
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            82789
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.415
_diffrn_reflns_theta_min         3.071
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    14.316
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41224
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       block
_exptl_crystal_F_000             3396
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.592
_refine_diff_density_min         -1.332
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1892
_refine_ls_number_reflns         27158
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.063
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+5.7694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1078
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24023
_reflns_number_total             27158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02687a2.cif
_cod_data_source_block           exp_311
_cod_database_code               7708512
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.52
_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. Uiso/Uaniso restraints and constraints
Uanis(O25) \\sim Ueq, Uanis(O26) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
3. Others
 Sof(H76C)=Sof(H76D)=Sof(H77C)=Sof(H77D)=Sof(S2A)=1-FVAR(1)
 Sof(S2)=Sof(H76A)=Sof(H76B)=Sof(H77A)=Sof(H77B)=FVAR(1)
 Sof(O25)=Sof(H25A)=Sof(H25B)=1-FVAR(2)
 Sof(O25A)=Sof(H25C)=Sof(H25D)=FVAR(2)
 Sof(O26A)=Sof(H26C)=Sof(H26D)=1-FVAR(3)
 Sof(O26)=Sof(H26A)=Sof(H26B)=FVAR(3)
 Fixed Sof: S6A(0.5) S6(0.5) H13C(0.5) H13D(0.5) H13A(0.5) H13B(0.5) H13G(0.5)
 H13H(0.5) H13E(0.5) H13F(0.5)
4.a Free rotating group:
 O27(H27A,H27B), O25(H25A,H25B), O26(H26A,H26B), O25A(H25C,H25D), O26A(H26C,
 H26D)
4.b Rotating group:
 O28(H28A,H28B)
4.c Secondary CH2 refined with riding coordinates:
 C149(H14A,H14B), C148(H14C,H14D), C61(H61A,H61B), C20(H20A,H20B), C60(H60A,
 H60B), C21(H21A,H21B), C76(H76A,H76B), C76(H76C,H76D), C77(H77A,H77B),
 C77(H77C,H77D), C133(H13C,H13D), C133(H13A,H13B), C117(H11A,H11B), C132(H13G,
 H13H), C132(H13E,H13F), C116(H11C,H11D)
4.d Aromatic/amide H refined with riding coordinates:
 C55(H55), C147(H147), C154(H154), C143(H143), C40(H40), C146(H146), C39(H39),
 C64(H64), C66(H66), C56(H56), C31(H31), C152(H152), C29(H29), C80(H80),
 C98(H98), C97(H97), C75(H75), C27(H27), C15(H15), C138(H138), C38(H38),
 C99(H99), C71(H71), C111(H111), C63(H63), C127(H127), C151(H151), C26(H26),
 C91(H91), C131(H131), C155(H155), C82(H82), C106(H106), C108(H108), C144(H144),
  C47(H47), C16(H16), C136(H136), C19(H19), C30(H30), C59(H59), C87(H87),
 C58(H58), C96(H96), C50(H50), C18(H18), C128(H128), C34(H34), C67(H67),
 C107(H107), C85(H85), C114(H114), C74(H74), C43(H43), C42(H42), C115(H115),
 C94(H94), C135(H135), C86(H86), C95(H95), C52(H52), C24(H24), C103(H103),
 C72(H72), C139(H139), C122(H122), C79(H79), C102(H102), C23(H23), C83(H83),
 C41(H41), C112(H112), C3(H3), C35(H35), C120(H120), C1(H1), C123(H123),
 C46(H46), C6(H6), C51(H51), C12(H12), C7(H7), C119(H119), C90(H90), C130(H130),
  C10(H10), C2(H2), C11(H11)
;
_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 3.357
_oxdiff_exptl_absorpt_empirical_full_min 0.456