Two series of Ln-MOFs by solvent induced self-assembly demonstrating the rapid selective sensing of Mg<sup>2+</sup> and Fe<sup>3+</sup> cations.
Wang, Xiaokang; Wang, Yutong; Wang, Xia; Lu, Kebin; Jiang, Weifeng; Cui, Pei-Pei; Hao, Hongguo; Dai, Fangna; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15473–15480; doi:10.1039/d0dt03264f

data_7706308
_publ_section_title
;
 Two series of Ln-MOFs by solvent induced self-assembly demonstrating the
 rapid selective sensing of Mg<sup>2+</sup> and Fe<sup>3+</sup> cations.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15473
_journal_page_last               15480
_journal_paper_doi               10.1039/d0dt03264f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C102 H65 Eu4 N9 O46, 0.5(O)'
_chemical_formula_sum            'C102 H65 Eu4 N9 O46.5'
_chemical_formula_weight         2768.47
_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
_audit_creation_date             2020-10-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-19 deposited with the CCDC.	2020-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                73.965(5)
_cell_angle_beta                 79.657(3)
_cell_angle_gamma                80.859(5)
_cell_formula_units_Z            1
_cell_length_a                   10.9059(5)
_cell_length_b                   15.0573(12)
_cell_length_c                   19.0395(6)
_cell_measurement_reflns_used    7103
_cell_measurement_temperature    297
_cell_measurement_theta_max      70.4090
_cell_measurement_theta_min      4.1520
_cell_volume                     2936.3(3)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      297.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.974
_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    -22.00  69.00   1.00    1.50    --    0.00  57.00   0.00   91
  2  \w    -46.00  17.00   1.00    1.50    --    0.00 103.00-122.00   63
  3  \w    -22.00  69.00   1.00    1.50    --    0.00  57.00 120.00   91
  4  \w     32.00 123.00   1.00    5.50    --   54.00  57.00-120.00   91
  5  \w     29.00  76.00   1.00    5.50    --   54.00 -57.00 -90.00   47
  6  \w     17.00  43.00   1.00    5.50    --   54.00 -99.00 -60.00   26
  7  \w     28.00 101.00   1.00    5.50    --   54.00-125.00-120.00   73
  8  \w    -15.00  60.00   1.00    5.50    --   54.00 -57.00  30.00   75
  9  \w     70.00  96.00   1.00    5.50    --   54.00 -99.00 -60.00   26
 10  \w     61.00 123.00   1.00    5.50    --   54.00  57.00-180.00   62
 11  \w    -12.00  80.00   1.00    5.50    --   54.00 -19.00-120.00   92
 12  \w     -5.00  68.00   1.00    5.50    --   54.00 -57.00  90.00   73
 13  \w     58.00 112.00   1.00    5.00    --  108.00-111.00-150.00   54
 14  \w     88.00 178.00   1.00    5.00    --  108.00  38.00  60.00   90
 15  \w     39.00  67.00   1.00    5.00    --  108.00 -38.00-120.00   28
 16  \w     36.00 111.00   1.00    5.00    --  108.00-111.00 -60.00   75
 17  \w     89.00 153.00   1.00    5.00    --  108.00  38.00 -30.00   64
 18  \w     44.00 105.00   1.00    5.00    --  108.00 -77.00 -60.00   61
 19  \w     71.00 103.00   1.00    5.00    --  108.00-111.00 150.00   32
 20  \w     70.00 111.00   1.00    5.00    --  108.00-111.00  60.00   41
 21  \w     44.00  70.00   1.00    5.00    --  108.00-111.00 150.00   26
 22  \w    150.00 176.00   1.00    5.00    --  108.00 111.00-150.00   26
 23  \w    109.00 167.00   1.00    5.00    --  108.00 111.00 -90.00   58
 24  \w     35.00 127.00   1.00    5.00    --  108.00 -38.00 120.00   92
 25  \w     74.00 126.00   1.00    5.00    --  108.00 178.00 -30.00   52
 26  \w     49.00 130.00   1.00    5.00    --  108.00 -50.00 -30.00   81
 27  \w     76.00 131.00   1.00    5.00    --  108.00 -38.00-120.00   55
 28  \w    103.00 177.00   1.00    5.00    --  108.00 -12.00  30.00   74
 29  \w     39.00  77.00   1.00    5.00    --  108.00 -12.00  30.00   38
 30  \w     87.00 112.00   1.00    5.50    --   54.00-125.00-150.00   25
 31  \w     56.00  81.00   1.00    5.50    --   54.00 -38.00   0.00   25
 32  \w    -12.00  14.00   1.00    5.50    --   54.00 -38.00   0.00   26
 33  \w    110.00 135.00   1.00    5.00    --  108.00 -38.00 -30.00   25
 34  \w     48.00  74.00   1.00    5.00    --  108.00 -38.00 -30.00   26
 35  \w     76.00 113.00   1.00    5.00    --  108.00 -63.00  60.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0149804000
_diffrn_orient_matrix_UB_12      -0.0214716000
_diffrn_orient_matrix_UB_13      0.0821522000
_diffrn_orient_matrix_UB_21      -0.0876587000
_diffrn_orient_matrix_UB_22      0.0890639000
_diffrn_orient_matrix_UB_23      0.0068052000
_diffrn_orient_matrix_UB_31      -0.1139718000
_diffrn_orient_matrix_UB_32      -0.0556121000
_diffrn_orient_matrix_UB_33      0.0209885000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23188
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.981
_diffrn_reflns_theta_min         4.148
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15623
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       block
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.933
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.00098(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         11062
_refine_ls_number_restraints     250
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0838
_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^)+(0.1334P)^2^+6.9119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2267
_refine_ls_wR_factor_ref         0.2575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7418
_reflns_number_total             11062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03264f2.cif
_cod_data_source_block           2-Eu
_cod_original_formula_sum        'C102 H65 Eu4 N9 O46.50'
_cod_database_code               7706308
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Eu'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(O1A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O20) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O1A)
\\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O2) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 N4, C46, C49, C48, C47, O20, Eu2, O19, O21, O11, O2, O1, O1A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N7, C57, C55, C56, O22, C54, O3, Eu1, O4, O23, C50, C51, N6, C52, C53
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: O1(0.5) N4(0.5) N6(0.5) N7(0.5) C46(0.5) H46A(0.5) H46B(0.5)
 H46C(0.5) C47(0.5) H47A(0.5) H47B(0.5) H47C(0.5) C48(0.5) C49(0.5) H49A(0.5)
 H49B(0.5) H49C(0.5) C50(0.5) C51(0.5) H51A(0.5) H51B(0.5) H51C(0.5) C52(0.5)
 H52A(0.5) H52B(0.5) H52C(0.5) C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5) C54(0.5)
 H54A(0.5) H54B(0.5) H54C(0.5) C55(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5)
 C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5) O1A(0.5) O24(0.25)
5.a Riding coordinates:
 O19(H19A,H19B), C49(H49A,H49B,H49C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
  C56(H56A,H56B,H56C), C57(H57A,H57B,H57C)
5.b Rotating group:
 O21(H21A,H21B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C10(H10), C11(H11), C16(H16), C17(H17), C19(H19), C22(H22),
 C28(H28), C31(H31), C36(H36), C38(H38), C41(H41), C42(H42), C43(H43)
5.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C51(H51A,H51B,H51C), C54(H54A,H54B,
 H54C)
;
_shelx_res_checksum              69351
_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 5.446
_oxdiff_exptl_absorpt_empirical_full_min 0.602