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_7706304
_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         'C23 H23 Eu N4 O11'
_chemical_formula_sum            'C23 H23 Eu N4 O11'
_chemical_formula_weight         683.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 102.649(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.4230(4)
_cell_length_b                   11.4174(3)
_cell_length_c                   34.1386(7)
_cell_measurement_reflns_used    6788
_cell_measurement_temperature    297
_cell_measurement_theta_max      70.5660
_cell_measurement_theta_min      4.0690
_cell_volume                     6245.9(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 0.994
_diffrn_measured_fraction_theta_max 0.977
_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    -36.00  -5.00   1.00    1.96    --    0.00 105.00 -74.00   31
  2  \w    -10.00  18.00   1.00    1.96    --    0.00  57.00 -60.00   28
  3  \w    -61.00 -34.00   1.00    1.96    --    0.00 135.00 178.00   27
  4  \w     27.00  69.00   1.00    1.96    --    0.00  57.00 -60.00   42
  5  \w     29.00  59.00   1.00    7.84    --   54.00-135.00 113.00   30
  6  \w     -8.00  72.00   1.00    7.84    --   54.00 -57.00 150.00   80
  7  \w    -20.00  94.00   1.00    7.84    --   54.00   0.00-180.00  114
  8  \w     24.00 100.00   1.00    7.84    --   54.00-125.00 150.00   76
  9  \w    105.00 156.00   1.00    7.84    --  108.00 105.00 -74.00   51
 10  \w    102.00 130.00   1.00    7.84    --  108.00  38.00 -90.00   28
 11  \w     98.00 176.00   1.00    7.84    --  108.00  38.00-180.00   78
 12  \w    100.00 160.00   1.00    7.84    --  108.00 111.00   0.00   60
 13  \w     48.00 112.00   1.00    7.84    --  108.00-111.00  90.00   64
 14  \w     39.00 134.00   1.00    7.84    --  108.00 -38.00   0.00   95
 15  \w     36.00 112.00   1.00    7.84    --  108.00-111.00-120.00   76
 16  \w     36.00  62.00   1.00    7.84    --  108.00-111.00-150.00   26
 17  \w     46.00 114.00   1.00    7.84    --  108.00 -77.00  90.00   68
;
_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      -0.0021463000
_diffrn_orient_matrix_UB_12      0.1116891000
_diffrn_orient_matrix_UB_13      0.0250705000
_diffrn_orient_matrix_UB_21      -0.0048620000
_diffrn_orient_matrix_UB_22      -0.0756633000
_diffrn_orient_matrix_UB_23      0.0367897000
_diffrn_orient_matrix_UB_31      0.0959883000
_diffrn_orient_matrix_UB_32      -0.0013419000
_diffrn_orient_matrix_UB_33      0.0125224000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            12127
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.538
_diffrn_reflns_theta_min         4.093
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.873
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35330
_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    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.668
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5839
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0636P)^2^+12.3839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5150
_reflns_number_total             5839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03264f2.cif
_cod_data_source_block           1-Eu
_cod_database_code               7706304
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Eu'
_reflns_odcompleteness_completeness 99.59
_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
2. Restrained distances
 N2-C23
 1.4 with sigma of 0.02
 C21A-C20A
 2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22A)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C23A) \\sim Ueq, Uanis(N2) \\sim Ueq,
Uanis(N2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N2, C20, C21, C22, N2A, C21A, C22A, C23, C20A, C23A, O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N2(0.5) C20(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C22(0.5)
 H22A(0.5) H22B(0.5) H22C(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C20A(0.5)
 N2A(0.5) C21A(0.5) H21D(0.5) H21E(0.5) H21F(0.5) C23A(0.5) H23D(0.5) H23E(0.5)
 H23F(0.5) C22A(0.5) H22D(0.5) H22E(0.5) H22F(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C14(H14), C15(H15)
6.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C21A(H21D,H21E,H21F),
 C23A(H23D,H23E,H23F), C22A(H22D,H22E,H22F)
;
_shelx_res_checksum              88283
_shelx_fab_checksum              90386
_platon_squeeze_void_probe_radius 1.20
_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 2.393
_oxdiff_exptl_absorpt_empirical_full_min 0.453