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_7706307
_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 H67 N9 O47 Sm4'
_chemical_formula_sum            'C102 H67 N9 O47 Sm4'
_chemical_formula_weight         2772.04
_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                74.153(5)
_cell_angle_beta                 79.198(5)
_cell_angle_gamma                80.098(5)
_cell_formula_units_Z            1
_cell_length_a                   10.9510(5)
_cell_length_b                   14.9310(9)
_cell_length_c                   19.1539(12)
_cell_measurement_reflns_used    8498
_cell_measurement_temperature    278.76(10)
_cell_measurement_theta_max      70.3020
_cell_measurement_theta_min      4.3700
_cell_volume                     2935.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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_environment      air
_diffrn_ambient_temperature      278.76(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_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    -69.00  22.00   1.00    1.50    --    0.00 -59.00  93.00   91
  2  \w    -69.00  22.00   1.00    1.50    --    0.00 -57.00  60.00   91
  3  \w    -22.00  69.00   1.00    1.50    --    0.00  57.00-150.00   91
  4  \w    -15.00  76.00   1.00    5.00    --   54.00 -57.00 150.00   91
  5  \w      1.00  98.00   1.00    5.00    --   54.00 -99.00-180.00   97
  6  \w     35.00 111.00   1.00    5.00    --   54.00-125.00 -30.00   76
  7  \w      6.00  72.00   1.00    5.00    --   54.00 -57.00  30.00   66
  8  \w    -19.00  99.00   1.00    5.00    --   54.00 -19.00-150.00  118
  9  \w     29.00 124.00   1.00    5.00    --   54.00  77.00   0.00   95
 10  \w     66.00 104.00   1.00    5.00    --   54.00  77.00  90.00   38
 11  \w     46.00 115.00   1.00    7.00    --  108.00-111.00-150.00   69
 12  \w     42.00 100.00   1.00    7.00    --  108.00-111.00  60.00   58
 13  \w     81.00 167.00   1.00    7.00    --  108.00  38.00 120.00   86
 14  \w     57.00  84.00   1.00    7.00    --  108.00-111.00-180.00   27
 15  \w     46.00 143.00   1.00    7.00    --  108.00 -25.00  60.00   97
 16  \w     81.00 148.00   1.00    7.00    --  108.00 178.00  60.00   67
 17  \w     90.00 115.00   1.00    7.00    --  108.00-111.00 -30.00   25
 18  \w     43.00  70.00   1.00    7.00    --  108.00-111.00 -30.00   27
 19  \w    104.00 172.00   1.00    7.00    --  108.00 111.00 120.00   68
 20  \w     82.00 118.00   1.00    7.00    --  108.00 178.00 -60.00   36
 21  \w    101.00 142.00   1.00    7.00    --  108.00 111.00  60.00   41
 22  \w    101.00 178.00   1.00    7.00    --  108.00 111.00  30.00   77
 23  \w    100.00 172.00   1.00    7.00    --  108.00 111.00   0.00   72
 24  \w     41.00 127.00   1.00    7.00    --  108.00 -25.00 -60.00   86
 25  \w     87.00 115.00   1.00    7.00    --  108.00-111.00  90.00   28
 26  \w     41.00 128.00   1.00    7.00    --  108.00 -64.00  30.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0460983000
_diffrn_orient_matrix_UB_12      -0.0856993000
_diffrn_orient_matrix_UB_13      0.0590645000
_diffrn_orient_matrix_UB_21      0.1319651000
_diffrn_orient_matrix_UB_22      0.0308146000
_diffrn_orient_matrix_UB_23      -0.0185434000
_diffrn_orient_matrix_UB_31      -0.0362138000
_diffrn_orient_matrix_UB_32      0.0583164000
_diffrn_orient_matrix_UB_33      0.0575755000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21559
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.438
_diffrn_reflns_theta_min         4.144
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.572
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             1366
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.541
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         10975
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0897P)^2^+10.6867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8894
_reflns_number_total             10975
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03264f2.cif
_cod_data_source_block           2-Sm
_cod_original_cell_volume        2935.1(3)
_cod_database_code               7706307
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.81
_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. Restrained distances
 C51-N6
 2.4 with sigma of 0.02
 C52-N6 = N6-C53
 1.4 with sigma of 0.02
 C50-C52 = C52-C53
 2.4 with sigma of 0.02
 N6-C50
 1.4 with sigma of 0.02
 C46-N4 = N4-C49
 1.4 with sigma of 0.02
 C48-C47
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N6) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53)
\\sim Ueq, Uanis(C51) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C54) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C55) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O1A) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Sm2, O20, N4, C46, C47, C48, C49
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O23, N6, C50, C51, C52, C53
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O22, N7, C54, C55, C56
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. 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) O26(0.5) H26A(0.5) H26B(0.5) O1A(0.5)
6.a Riding coordinates:
 O19(H19A,H19B), O21(H21A,H21B), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C),
 O26(H26A,H26B)
6.b 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)
6.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C52(H52A,H52B,
 H52C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C)
;
_shelx_res_checksum              592
_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 2.553
_oxdiff_exptl_absorpt_empirical_full_min 0.634