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_7706306
_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 N4 Nd O11'
_chemical_formula_sum            'C23 H23 N4 Nd O11'
_chemical_formula_weight         675.69
_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   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                90
_cell_angle_beta                 102.1983(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.5848(3)
_cell_length_b                   11.5280(3)
_cell_length_c                   33.9909(7)
_cell_measurement_reflns_used    6605
_cell_measurement_temperature    297.0
_cell_measurement_theta_max      70.4030
_cell_measurement_theta_min      4.0420
_cell_volume                     6352.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (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 0.997
_diffrn_measured_fraction_theta_max 0.981
_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    -14.00  13.00   1.00    1.00    --    0.00  57.00  60.00   27
  2  \w     17.00  69.00   1.00    1.00    --    0.00  57.00  60.00   52
  3  \w    -35.00   7.00   1.00    1.00    --    0.00 100.00-135.00   42
  4  \w    -59.00 -33.00   1.00    1.00    --    0.00 138.00 113.00   26
  5  \w     63.00 120.00   1.00    2.06    --   53.47  77.00 150.00   57
  6  \w     44.00  81.00   1.00    2.06    --   53.47 -77.00  90.00   37
  7  \w      2.00  96.00   1.00    2.06    --   53.47 -99.00  30.00   94
  8  \w    -15.00  12.00   1.00    2.06    --   53.47 -77.00  60.00   27
  9  \w     26.00  97.00   1.00    2.06    --   53.47  38.00 150.00   71
 10  \w    -16.00  14.00   1.00    2.06    --   53.47 -77.00  90.00   30
 11  \w     39.00 111.00   1.00    2.06    --  106.95-111.00-150.00   72
 12  \w     93.00 157.00   1.00    2.06    --  106.95  63.00 150.00   64
 13  \w     84.00 112.00   1.00    2.06    --  106.95-111.00  60.00   28
 14  \w    127.00 178.00   1.00    2.06    --  106.95 111.00   0.00   51
 15  \w     59.00 131.00   1.00    2.06    --  106.95 -63.00-180.00   72
 16  \w    101.00 156.00   1.00    2.06    --  106.95 100.00-135.00   55
 17  \w    106.00 164.00   1.00    2.06    --  106.95 111.00  90.00   58
 18  \w     34.00 101.00   1.00    2.06    --  106.95-111.00  30.00   67
 19  \w     85.00 177.00   1.00    2.06    --  106.95  77.00 -90.00   92
;
_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      0.0102063000
_diffrn_orient_matrix_UB_12      -0.0189350000
_diffrn_orient_matrix_UB_13      -0.0435486000
_diffrn_orient_matrix_UB_21      0.0004799000
_diffrn_orient_matrix_UB_22      -0.1322477000
_diffrn_orient_matrix_UB_23      0.0065299000
_diffrn_orient_matrix_UB_31      -0.0944984000
_diffrn_orient_matrix_UB_32      -0.0027608000
_diffrn_orient_matrix_UB_33      -0.0145238000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            12424
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.466
_diffrn_reflns_theta_min         4.059
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.962
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (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    1.413
_exptl_crystal_description       block
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.984
_refine_diff_density_min         -2.224
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5960
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0728
_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^)+(0.1742P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2117
_refine_ls_wR_factor_ref         0.2228
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5147
_reflns_number_total             5960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03264f2.cif
_cod_data_source_block           1-Nd
_cod_database_code               7706306
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Nd'
_reflns_odcompleteness_completeness 99.61
_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 C(H,H,H,H,H,H) groups
2. Restrained distances
 N2-C23
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(N2)
\\sim Ueq, Uanis(N2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(N2A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 O7, N2, N2A, C20, C20A, C21, C22, C23
 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) N2A(0.5) C20(0.5) C20A(0.5) H21A(0.5) H21B(0.5) H21C(0.5)
 H21D(0.5) H21E(0.5) H21F(0.5) H22A(0.5) H22B(0.5) H22C(0.5) H22D(0.5)
 H22E(0.5) H22F(0.5) H23A(0.5) H23B(0.5) H23C(0.5) H23D(0.5) H23E(0.5) H23F(0.5)
6.a Riding coordinates:
 C21(H21A,H21B,H21C), C21(H21D,H21E,H21F), C22(H22A,H22B,H22C), C22(H22D,H22E,
 H22F), C23(H23A,H23B,H23C), C23(H23D,H23E,H23F)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C14(H14), C15(H15)
6.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              5572
_shelx_fab_checksum              1593
_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 2.103
_oxdiff_exptl_absorpt_empirical_full_min 0.471