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_7708511
_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 Pr4 S6, H2 O, C12 H8 N2'
_chemical_formula_sum            'C156 H116 N10 O26 Pr4 S6'
_chemical_formula_weight         3302.58
_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
_audit_creation_date             2019-06-08
_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                70.7540(10)
_cell_angle_beta                 89.2320(10)
_cell_angle_gamma                80.4290(10)
_cell_formula_units_Z            2
_cell_length_a                   11.6366(2)
_cell_length_b                   22.1801(3)
_cell_length_c                   29.5908(3)
_cell_measurement_reflns_used    30358
_cell_measurement_temperature    296.8(7)
_cell_measurement_theta_max      73.9270
_cell_measurement_theta_min      3.8140
_cell_volume                     7103.17(18)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.8(7)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9944
_diffrn_measured_fraction_theta_max 0.9617
_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     28.00  71.00   0.50    2.50    --    0.00  57.00 -30.00   86
  2  \w    -89.00  31.00   0.50    2.50    --    0.00 -38.00  90.00  240
  3  \w     38.00  66.00   0.50    2.50    --    0.00  57.00   0.00   56
  4  \w    -29.00   9.00   0.50    2.50    --    0.00  57.00 -30.00   76
  5  \w    -29.00  87.00   0.50    2.50    --    0.00  38.00  90.00  232
  6  \w     71.00 150.00   0.50   22.00    --   95.80  30.00-150.00  158
  7  \w     19.00  68.00   0.50   22.00    --   95.80 -77.00  90.00   98
  8  \w     12.00 117.00   0.50   22.00    --   95.80 -61.00 120.00  210
  9  \w     91.00 123.00   0.50   22.00    --   95.80 -82.00-180.00   64
 10  \w    101.00 126.00   0.50   22.00    --   95.80 -45.00  60.00   50
 11  \w     72.00 162.00   0.50   22.00    --   95.80  45.00 -90.00  180
 12  \w      8.00  71.00   0.50   22.00    --   95.80 -30.00 -60.00  126
 13  \w     75.00 116.00   0.50   22.00    --   95.80 -30.00 -60.00   82
 14  \w     57.00 132.00   0.50   22.00    --   95.80 -82.00   0.00  150
 15  \w     59.00 102.00   0.50   22.00    --   95.80 -82.00  60.00   86
 16  \w     36.00 130.00   0.50   22.00    --   95.80 -82.00 120.00  188
 17  \w     37.00 133.00   0.50   22.00    --   95.80 -82.00 -90.00  192
 18  \w     13.00  39.00   0.50   22.00    --   95.80 -45.00  60.00   52
 19  \w      8.00 126.00   0.50   22.00    --   95.80 -45.00 -60.00  236
 20  \w     72.00  98.00   0.50   22.00    --   95.80 -82.00-120.00   52
 21  \w      8.00  73.00   0.50   22.00    --   95.80 -77.00 -60.00  130
 22  \w     71.00 181.00   0.50   22.00    --   95.80  45.00-120.00  220
;
_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      0.0421545000
_diffrn_orient_matrix_UB_12      0.0511836000
_diffrn_orient_matrix_UB_13      0.0174281000
_diffrn_orient_matrix_UB_21      -0.0204802000
_diffrn_orient_matrix_UB_22      -0.0396255000
_diffrn_orient_matrix_UB_23      0.0521106000
_diffrn_orient_matrix_UB_31      0.1259538000
_diffrn_orient_matrix_UB_32      -0.0372328000
_diffrn_orient_matrix_UB_33      0.0052593000
_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  0.0635
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            79542
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.574
_diffrn_reflns_theta_min         3.057
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    11.779
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51521
_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    1.544
_exptl_crystal_description       block
_exptl_crystal_F_000             3324
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.283
_refine_diff_density_min         -2.275
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1837
_refine_ls_number_reflns         28000
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0630
_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^)+(0.1199P)^2^+1.9771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1825
_refine_ls_wR_factor_ref         0.1963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20660
_reflns_number_total             28000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02687a2.cif
_cod_data_source_block           pr
_cod_database_code               7708511
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.44
_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
 C65-S6 \\sim S6-C64
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S6: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(S6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(S1A) = Uanis(S1)
4. Others
 Sof(H21c)=Sof(H21d)=Sof(H20c)=Sof(H20d)=Sof(S1)=1-FVAR(1)
 Sof(S1A)=Sof(H21a)=Sof(H21b)=Sof(H20a)=Sof(H20b)=FVAR(1)
 Sof(H04c)=Sof(H04d)=Sof(H79c)=Sof(H79d)=Sof(S3A)=1-FVAR(2)
 Sof(S3)=Sof(H04a)=Sof(H04b)=Sof(H79a)=Sof(H79b)=FVAR(2)
5.a Free rotating group:
 O25(H25a,H25b)
5.b Rotating group:
 O15(H26a,H26b)
5.c Secondary CH2 refined with riding coordinates:
 C36(H36a,H36b), C37(H37a,H37b), C95(H95a,H95b), C21(H21a,H21b), C21(H21c,
 H21d), C04T(H04a,H04b), C04T(H04c,H04d), C20(H20a,H20b), C20(H20c,H20d),
 C94(H94a,H94b), C65(H65a,H65b), C147(H14a,H14b), C79(H79a,H79b), C79(H79c,
 H79d), C64(H64a,H64b), C146(H14c,H14d)
5.d Aromatic/amide H refined with riding coordinates:
 C100(H100), C89(H89), C138(H138), C35(H35), C101(H101), C127(H127), C78(H78),
 C26(H26), C34(H34), C45(H45), C59(H59), C42(H42), C137(H137), C82(H82),
 C74(H74), C31(H31), C54(H54), C15(H15), C93(H93), C32(H32), C153(H153),
 C136(H136), C56(H56), C27(H27), C129(H129), C141(H141), C24(H24), C97(H97),
 C12(H12), C90(H90), C81(H81), C84(H84), C47(H47), C142(H142), C16(H16),
 C63(H63), C92(H92), C132(H132), C19(H19), C55(H55), C39(H39), C98(H98),
 C43(H43), C40(H40), C85(H85), C145(H145), C112(H112), C62(H62), C152(H152),
 C23(H23), C18(H18), C125(H125), C6(H6), C128(H128), C51(H51), C108(H108),
 C77(H77), C115(H115), C70(H70), C117(H117), C10(H10), C1(H1), C109(H109),
 C120(H120), C50(H50), C133(H133), C75(H75), C60(H60), C150(H150), C124(H124),
 C46(H46), C11(H11), C67(H67), C116(H116), C149(H149), C2(H2), C121(H121),
 C71(H71), C68(H68), C114(H114), C126(H126), C3(H3), C144(H144), C103(H103),
 C7(H7), C105(H105), C113(H113), C104(H104)
;
_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 2.422
_oxdiff_exptl_absorpt_empirical_full_min 0.450