Lanthanide-based bis-(3,5-dicarboxy-phenyl)terephthalamide metal‒organic frameworks: slow relaxation of magnetization and detection of trace Fe2+ and Fe3+
Lin, Qingfang; Xie, Wen; Zong, Zhihui; Liu, Zicheng; Sun, Yuqing; Liang, Lili; New Journal of Chemistry 45 (2021) 7382–7389; doi:10.1039/D1NJ00863C

data_7060461
_publ_section_title
;
 Lanthanide-based bis-(3,5-dicarboxy-phenyl)terephthalamide metal--organic
 frameworks: slow relaxation of magnetization and detection of trace Fe2+
 and Fe3+
;
_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7382
_journal_page_last               7389
_journal_paper_doi               10.1039/D1NJ00863C
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C48 H46 Dy2 N7 O19, H2 O'
_chemical_formula_sum            'C48 H48 Dy2 N7 O20'
_chemical_formula_weight         1367.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-04-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.07.08 svn.r3312 for OlexSys, GUI svn.r5203)
;
_audit_update_record
;
2018-10-22 deposited with the CCDC.	2021-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.535(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.681(2)
_cell_length_b                   21.1352(9)
_cell_length_c                   19.0189(10)
_cell_measurement_temperature    173(2)
_cell_volume                     14744.0(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            53469
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.396
_diffrn_reflns_theta_max         25.396
_diffrn_reflns_theta_min         2.868
_exptl_absorpt_coefficient_mu    2.071
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_F_000             5416
_refine_diff_density_max         2.824
_refine_diff_density_min         -1.996
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         13476
_refine_ls_number_restraints     2137
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1342
_refine_ls_R_factor_gt           0.0787
_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^)+(0.1076P)^2^+427.6729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1940
_refine_ls_wR_factor_ref         0.2428
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8117
_reflns_number_total             13476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00863c2.cif
_cod_data_source_block           Liang1
_cod_depositor_comments
'Adding full bibliography for 7060461--7060462.cif.'
_cod_database_code               7060461
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C19-C20
 2.5 with sigma of 0.01
 C24-C22
 2.5 with sigma of 0.01
 C24-C23
 2.5 with sigma of 0.01
 C11_$1-C10_$1 = C12_$1-C11_$1 = C10_$1-C10 = C11-C10 = C12-C11 = C12_$1-C12
 1.45 with sigma of 0.01
 C21-C19
 2.5 with sigma of 0.01
 O9-C24A
 1.2 with sigma of 0.01
 N4A-C24A = N4A-C23A = N4A-C22A
 1.5 with sigma of 0.01
 C24A-C22A
 2.5 with sigma of 0.01
 C24A-C23A
 2.5 with sigma of 0.01
 O6-C13A
 1.2 with sigma of 0.01
 C13A-C15A
 2.5 with sigma of 0.01
 C13A-C14A
 2.5 with sigma of 0.01
 O8-C19A
 1.2 with sigma of 0.01
 C19A-C20A
 2.5 with sigma of 0.01
 N5A-C19A = N5A-C20A = N5A-C21A
 1.5 with sigma of 0.01
 C19A-C21A
 2.5 with sigma of 0.01
 N2A-C13A = N2A-C14A = N2A-C15A
 1.5 with sigma of 0.01
 O9-C24 = O8-C19 = O6-C13 = O7-C16
 1.2 with sigma of 0.01
 O6-N2
 2.2 with sigma of 0.01
 Dy2-C13
 3.1 with sigma of 0.01
 C14-C15
 2.5 with sigma of 0.01
 C15-C14
 2.5 with sigma of 0.01
 C13-C15
 2.5 with sigma of 0.01
 N4-C23 = N4-C22 = N4-C24 = N5-C19 = N5-C21 = N5-C20 = N2-C13 = N2-C14 = N2-
 C15 = N3-C17 = N3-C18 = N3-C16
 1.5 with sigma of 0.01
 N7-C53 \\sim N6-C31 \\sim N6-C29
 with sigma of 0.02
 C54-C52 \\sim C33-C30
 with sigma of 0.02
 N7-C52 \\sim N6-C30
 with sigma of 0.02
 O15-N7 \\sim O14-N6
 with sigma of 0.02
 N7-C55 \\sim N6-C34
 with sigma of 0.02
 O15-C55 \\sim O14-C34
 with sigma of 0.02
 C54-N7 \\sim C33-N6
 with sigma of 0.02
 C54-O15 \\sim C33-O14
 with sigma of 0.02
 C54-C56 \\sim C33-C39 \\sim C33-C35
 with sigma of 0.02
 C55-C54 \\sim C34-C33
 with sigma of 0.02
 N7-C53 \\sim N8-C42 \\sim N8-C64
 with sigma of 0.02
 C54-C52 \\sim C40-C41
 with sigma of 0.02
 N7-C52 \\sim N8-C41
 with sigma of 0.02
 O15-N7 \\sim O16-N8
 with sigma of 0.02
 N7-C55 \\sim N8-C37
 with sigma of 0.02
 O15-C55 \\sim O16-C37
 with sigma of 0.02
 C54-N7 \\sim C40-N8
 with sigma of 0.02
 C54-O15 \\sim C40-O16
 with sigma of 0.02
 C54-C56 \\sim C40-C36 \\sim C40-C38
 with sigma of 0.02
 C55-C54 \\sim C37-C40
 with sigma of 0.02
 N7-C53 \\sim N7-C51 \\sim N9-C68 \\sim N9-C63
 with sigma of 0.02
 C54-C52 \\sim C61-C62
 with sigma of 0.02
 N7-C52 \\sim N9-C62
 with sigma of 0.02
 O15-N7 \\sim O17-N9
 with sigma of 0.02
 N7-C55 \\sim N9-C58
 with sigma of 0.02
 O15-C55 \\sim O17-C58
 with sigma of 0.02
 C54-N7 \\sim C61-N9
 with sigma of 0.02
 C54-O15 \\sim C61-O17
 with sigma of 0.02
 C54-C56 \\sim C54-C60 \\sim C61-C59 \\sim C61-C57
 with sigma of 0.02
 C55-C54 \\sim C58-C61
 with sigma of 0.02
3. Restrained planarity
 N8, C41, C42, C43, C66, C65, C64
 with sigma of 0.1
 N6, C30, C31, C26, C27, C28, C29
 with sigma of 0.1
 C37, C40, N8, O16
 with sigma of 0.1
 C34, C33, N6, O14
 with sigma of 0.1
 N9, C62, C68, C67, C44, C45, C63
 with sigma of 0.1
 N7, C52, C53, C48, C49, C50, C51
 with sigma of 0.1
 C58, C61, N9, O17
 with sigma of 0.1
 C55, C54, N7, O15
 with sigma of 0.1
 N5, C21, C19, O8, C20
 with sigma of 0.01
 C16, C18, C17, N3, O7
 with sigma of 0.01
 C24, N4, O9, C22, C23
 with sigma of 0.01
 O9, C24A, C22A, C23A, N4A
 with sigma of 0.01
 O8, C19A, C20A, C21A, N5A
 with sigma of 0.01
 O6, C13A, C15A, C14A, N2A
 with sigma of 0.01
 C13, N2, C15, O6, C14
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C48 \\sim C26 \\sim C49 \\sim C27 \\sim C50 \\sim C28 \\sim C51 \\sim C29 \\sim
C52 \\sim C30 \\sim N6 \\sim N7 \\sim C54 \\sim C33 \\sim O15 \\sim O14 \\sim
C34 \\sim C39 \\sim C38 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim C55 \\sim
C35 \\sim C36 \\sim C56 \\sim C37 \\sim C40 \\sim C61 \\sim O17 \\sim O16 \\sim
N8 \\sim N9 \\sim C62 \\sim C41 \\sim C63 \\sim C64 \\sim C45 \\sim C65 \\sim
C44 \\sim C66 \\sim C67 \\sim C43 \\sim C68 \\sim C42: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C24 \\sim N4 \\sim O9 \\sim C22 \\sim C23 \\sim C24A \\sim N4A \\sim C23A \\sim
C22A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N5 \\sim C21 \\sim C19 \\sim O8 \\sim C20 \\sim N5A \\sim C21A \\sim C19A \\sim
C20A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C13 \\sim N2 \\sim C15 \\sim O6 \\sim C14 \\sim C13A \\sim N2A \\sim C15A \\sim
C14A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(N5)
\\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C24) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C23)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C48) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C51) \\sim Ueq,
Uanis(C29) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(N6)
\\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C33) \\sim Ueq,
Uanis(O15) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq,
Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C37) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O16)
\\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(C62) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C66) \\sim Ueq,
Uanis(C67) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C42)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C53) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(N1) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O22) \\sim Ueq, Uanis(O23) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C24) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(N4A) \\sim Ueq,
Uanis(C23A) \\sim Ueq, Uanis(C22A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N5) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(O8)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(N5A) \\sim Ueq, Uanis(C21A) \\sim Ueq,
Uanis(C19A) \\sim Ueq, Uanis(C20A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O6) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(O6)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(N2A) \\sim Ueq,
Uanis(C15A) \\sim Ueq, Uanis(C14A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O23) = Uanis(O22)
5. Rigid body (RIGU) restrains
 C48, C26, C49, C27, C50, C28, C51, C29, C52, C30, N6, N7, C54, C33, O15, O14,
 C34, C39, C38, C57, C58, C59, C60, C55, C35, C36, C56, C37, C40, C61, O17, O16,
  N8, N9, C62, C41, C63, C64, C45, C65, C44, C66, C67, C43, C68, C42
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C24, N4, O9, C22, C23, C24A, N4A, C23A, C22A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N5, C21, C19, O8, C20, N5A, C21A, C19A, C20A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13, N2, C15, H12, O6, C14, C13A, N2A, C15A, C14A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(C34)=Sof(C39)=Sof(H39)=Sof(C38)=Sof(H38)=Sof(C37)=Sof(C36)=Sof(H36)=
 Sof(C35)=Sof(H35)=Sof(C33)=Sof(N6)=Sof(H6)=Sof(O14)=Sof(C30)=Sof(C31)=Sof(H31)=
 Sof(C26)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(C29)=Sof(H29)=Sof(C40)=Sof(N8)=Sof(H8)=
 Sof(O16)=Sof(C41)=Sof(C42)=Sof(H42)=Sof(C43)=Sof(C66)=Sof(H66)=Sof(C65)=
 Sof(C64)=Sof(H64)=1-FVAR(1)
 Sof(C55)=Sof(C56)=Sof(H56)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(C59)=Sof(H59)=
 Sof(C60)=Sof(H60)=Sof(C54)=Sof(N7)=Sof(H7A)=Sof(O15)=Sof(C52)=Sof(C53)=
 Sof(H53)=Sof(C48)=Sof(C49)=Sof(H49)=Sof(C50)=Sof(C51)=Sof(H51)=Sof(C61)=
 Sof(N9)=Sof(H9)=Sof(O17)=Sof(C62)=Sof(C68)=Sof(H68)=Sof(C67)=Sof(C44)=Sof(H44)=
 Sof(C45)=Sof(C63)=Sof(H63)=FVAR(1)
 Sof(C24A)=Sof(H24A)=Sof(N4A)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=
 Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(2)
 Sof(C24)=Sof(H24)=Sof(N4)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=
 Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(2)
 Sof(C13A)=Sof(H13A)=Sof(N2A)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=
 Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(3)
 Sof(C13)=Sof(H13)=Sof(N2)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C14)=
 Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(3)
 Sof(N5A)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C19A)=Sof(H19A)=
 Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(4)
 Sof(N5)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C19)=Sof(H19)=Sof(C20)=
 Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(4)
 Fixed Sof: O22(0.5) H22G(0.5) H22H(0.5) O23(0.5) H23G(0.5) H23H(0.5)
7.a Riding coordinates:
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), O22(H22G,H22H), O23(H23G,H23H),
 C21A(H21D,H21E,H21F)
7.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C19(H19), C24(H24), C12(H12), C10(H10), C5(H5), C3(H3), C7(H7),
 C16(H16), N1(H1), C56(H56), C57(H57), C59(H59), C60(H60), N7(H7A), C53(H53),
 C49(H49), C51(H51), N9(H9), C68(H68), C44(H44), C63(H63), C39(H39), C38(H38),
 C36(H36), C35(H35), N6(H6), C31(H31), C27(H27), C29(H29), N8(H8), C42(H42),
 C66(H66), C64(H64), C24A(H24A), C13A(H13A), C19A(H19A)
7.c Fitted hexagon refined as free rotating group:
 C55(C56,C57,C58,C59,C60), C52(C53,C48,C49,C50,C51), C62(C68,C67,C44,C45,C63),
 C34(C39,C38,C37,C36,C35), C30(C31,C26,C27,C28,C29), C41(C42,C43,C66,C65,C64)
7.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C23A(H23D,H23E,H23F),
 C22A(H22D,H22E,H22F), C15A(H15D,H15E,H15F), C14A(H14D,H14E,H14F), C20A(H20D,
 H20E,H20F)
;
_shelx_res_checksum              61452
_shelx_fab_checksum              95448
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'