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_7708514
_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 Ce4 N8 O25 S6, 3(H2 O), C12 H8 N2'
_chemical_formula_sum            'C156 H120 Ce4 N10 O28 S6'
_chemical_formula_weight         3335.45
_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             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                71.0700(10)
_cell_angle_beta                 89.0760(10)
_cell_angle_gamma                80.4440(10)
_cell_formula_units_Z            2
_cell_length_a                   11.58490(10)
_cell_length_b                   22.0997(2)
_cell_length_c                   29.3064(3)
_cell_measurement_reflns_used    76162
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.0460
_cell_measurement_theta_min      3.8380
_cell_volume                     6993.09(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 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      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.972
_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    -89.00  32.00   0.50    1.37    --    0.00 -38.00 -90.00  242
  2  \w    -89.00  30.00   0.50    1.37    --    0.00 -57.00-180.00  238
  3  \w    -35.00  89.00   0.50    1.37    --    0.00  77.00  30.00  248
  4  \w    -89.00  32.00   0.50    1.37    --    0.00 -38.00 -90.00  242
  5  \w      6.00 133.00   0.50    6.00    --   95.80 -82.00  60.00  254
  6  \w      6.00 126.00   0.50    6.00    --   95.80 -61.00   0.00  240
  7  \w      6.00 126.00   0.50    6.00    --   95.80 -45.00-150.00  240
  8  \w     58.00 185.00   0.50    6.00    --   95.80  82.00 150.00  254
  9  \w     63.00 185.00   0.50    6.00    --   95.80  39.00  75.56  244
 10  \w      6.00 133.00   0.50    6.00    --   95.80 -82.00 -60.00  254
 11  \w      6.00 133.00   0.50    6.00    --   95.80 -82.00   0.00  254
 12  \w      6.00 133.00   0.50    6.00    --   95.80 -82.00 120.00  254
 13  \w      6.00 132.00   0.50    6.00    --   95.80 -30.00  30.00  252
 14  \w      6.00 126.00   0.50    6.00    --   95.80 -61.00-150.00  240
 15  \w      6.00 133.00   0.50    6.00    --   95.80 -82.00-150.00  254
 16  \w      6.00 133.00   0.50    6.00    --   95.80 -82.00-120.00  254
 17  \w      6.00 185.00   0.50    6.00    --   95.80  15.00 150.00  358
 18  \w    -30.00  89.00   0.50    1.37    --    0.00  57.00 120.00  238
 19  \w    -89.00  35.00   0.50    1.37    --    0.00 -77.00 -60.00  248
 20  \w    -89.00  35.00   0.50    1.37    --    0.00 -77.00 -30.00  248
 21  \w    -56.00  53.00   0.50    1.37    --    0.00  19.00 120.00  218
 22  \w    -89.00  30.00   0.50    1.37    --    0.00 -57.00  60.00  238
;
_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      0.1122183000
_diffrn_orient_matrix_UB_12      0.0170810000
_diffrn_orient_matrix_UB_13      0.0166427000
_diffrn_orient_matrix_UB_21      0.0373148000
_diffrn_orient_matrix_UB_22      0.0230286000
_diffrn_orient_matrix_UB_23      -0.0527076000
_diffrn_orient_matrix_UB_31      -0.0650327000
_diffrn_orient_matrix_UB_32      0.0690691000
_diffrn_orient_matrix_UB_33      -0.0061922000
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            135072
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.495
_diffrn_reflns_theta_min         3.063
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    11.353
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55886
_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    1.584
_exptl_crystal_description       block
_exptl_crystal_F_000             3356
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.289
_refine_diff_density_min         -1.638
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1900
_refine_ls_number_reflns         27833
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0554P)^2^+7.7609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.0977
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25752
_reflns_number_total             27833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02687a2.cif
_cod_data_source_block           ce-2
_cod_original_cell_volume        6993.10(12)
_cod_database_code               7708514
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.65
_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. Others
 Sof(S4A)=Sof(H64C)=Sof(H64D)=Sof(H65C)=Sof(H65D)=1-FVAR(1)
 Sof(S4)=Sof(H64A)=Sof(H64B)=Sof(H65A)=Sof(H65B)=FVAR(1)
 Sof(O2X)=Sof(H2XA)=Sof(H2XB)=1-FVAR(2)
 Sof(O2W)=Sof(H2WA)=Sof(H2WB)=FVAR(2)
 Fixed Sof: S5(0.5) S5A(0.5) C95A(0.5) H95A(0.5) H95B(0.5) C95(0.5) H95C(0.5)
 H95D(0.5) H96C(0.5) H96D(0.5) H96A(0.5) H96B(0.5) O3W(0.5) H3WA(0.5) H3WB(0.5)
 O3X(0.5) H3XA(0.5) H3XB(0.5)
3.a Free rotating group:
 O4W(H4WA,H4WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O2X(H2XA,H2XB), O3X(H3XA,H3XB)
3.b Rotating group:
 O1W(H1WA,H1WB)
3.c Secondary CH2 refined with riding coordinates:
 C95A(H95A,H95B), C20(H20A,H20B), C21(H21A,H21B), C36(H36A,H36B), C37(H37A,
 H37B), C64(H64A,H64B), C64(H64C,H64D), C65(H65A,H65B), C65(H65C,H65D),
 C80(H80A,H80B), C81(H81A,H81B), C95(H95C,H95D), C96(H96C,H96D), C96(H96A,H96B),
  C111(H11A,H11B), C112(H11C,H11D)
3.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C18(H18), C19(H19), C23(H23), C24(H24), C26(H26), C27(H27),
  C31(H31), C32(H32), C34(H34), C35(H35), C39(H39), C40(H40), C42(H42),
 C43(H43), C45(H45), C46(H46), C47(H47), C52(H52), C53(H53), C54(H54), C55(H55),
  C56(H56), C59(H59), C60(H60), C62(H62), C63(H63), C67(H67), C68(H68),
 C70(H70), C71(H71), C75(H75), C76(H76), C78(H78), C79(H79), C83(H83), C84(H84),
  C86(H86), C87(H87), C90(H90), C91(H91), C93(H93), C94(H94), C98(H98),
 C99(H99), C101(H101), C102(H102), C106(H106), C107(H107), C109(H109),
 C110(H110), C114(H114), C115(H115), C117(H117), C118(H118), C120(H120),
 C121(H121), C122(H122), C125(H125), C126(H126), C129(H129), C130(H130),
 C131(H131), C132(H132), C133(H133), C134(H134), C137(H137), C138(H138),
 C141(H141), C142(H142), C143(H143), C144(H144), C145(H145), C146(H146),
 C148(H148), C149(H149), C152(H152), C153(H153), C154(H154)
;
_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 3.116
_oxdiff_exptl_absorpt_empirical_full_min 0.462