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_7060462
_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 N7 O19 Sm2'
_chemical_formula_sum            'C48 H46 N7 O19 Sm2'
_chemical_formula_weight         1325.64
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-04
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2018-10-22 deposited with the CCDC.	2021-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.864(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.6398(14)
_cell_length_b                   21.2459(9)
_cell_length_c                   19.1182(9)
_cell_measurement_temperature    293(2)
_cell_volume                     14880.8(11)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            60727
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         25.391
_diffrn_reflns_theta_min         2.890
_exptl_absorpt_coefficient_mu    1.620
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_F_000             5271
_platon_squeeze_details          TITL
_refine_diff_density_max         3.018
_refine_diff_density_min         -1.411
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         13631
_refine_ls_number_restraints     1259
_refine_ls_restrained_S_all      Infinity
_refine_ls_R_factor_all          0.1139
_refine_ls_R_factor_gt           0.0703
_refine_ls_shift/su_max          0.135
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1099P)^2^+268.1089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1806
_refine_ls_wR_factor_ref         0.2191
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8803
_reflns_number_total             13631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00863c2.cif
_cod_data_source_block           Liang2
_cod_depositor_comments
'Adding full bibliography for 7060461--7060462.cif.'
_cod_database_code               7060462
_shelx_shelxl_version_number     2014/7
_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
2. Restrained distances
 C15-C17
 2.5 with sigma of 0.01
 C16A-C15A = C16-C15 = C20-C19 = C20A-C19A
 1.45 with sigma of 0.01
 C18A-C20A
 2.5 with sigma of 0.01
 O21A-N2A
 2.2 with sigma of 0.01
 N2-O21
 2.2 with sigma of 0.01
 O10A-C16A
 2.4 with sigma of 0.01
 O22-C44
 1.2 with sigma of 0.01
 O22-N4
 2.4 with sigma of 0.01
 C44-C45
 2.5 with sigma of 0.01
 C45-C46
 2.5 with sigma of 0.01
 C46-C44
 2.5 with sigma of 0.01
 C43A-C42A
 2.5 with sigma of 0.01
 N7A-C15 = O16-C20 = O10-C15 = N6-C20
 1.2 with sigma of 0.01
 N7A-C14 = N7-C14 = N6-C21 = N6A-C21
 1.45 with sigma of 0
 N7-C14 = N7A-C14 = N6-C21 = N6A-C21
 1.45 with sigma of 0.01
 O10A-C15A = O10-C15 = N7A-C15 = N7-C15A = N6-C20 = O16-C20 = O16A-C20A = N6A-
 C20A
 1.3 with sigma of 0.01
 O4-N3
 2.23 with sigma of 0.01
 O20A-C38A = O20-C38
 1.2 with sigma of 0.01
 N5-C38 = N5A-C38A = N5-C47 = N5A-C47A = N5-C39 = N5A-C39A
 1.5 with sigma of 0.01
 C38-C47
 2.5 with sigma of 0.01
 C47A-C38A
 2.5 with sigma of 0.01
 C39-C47
 2.5 with sigma of 0.01
 C47A-C39A
 2.5 with sigma of 0.01
 O21-C41
 1.2 with sigma of 0.01
 O21A-C41A = O21-C41
 1.2 with sigma of 0.01
 C43-C42
 2.5 with sigma of 0.01
 C42-C41 = C43-C41
 2.5 with sigma of 0.01
 N2-C41 = N2A-C41A = N2A-C43A = N2A-C42A = N2-C42 = N2-C43
 1.5 with sigma of 0.01
 N1-C37 = N1-C36 = N1-C35 = N5-C38 = N5-C47 = N5-C39 = N2-C43 = N2-C42 = N2-
 C41 = N4-C44 = N4-C45 = N4-C46
 1.5 with sigma of 0.01
3. Restrained planarity
 C15, C16, C30, C29, C19, C17, C18, C20
 with sigma of 0.01
 C15A, C16A, C30A, C17A, C18A, C29A, C19A, C20A
 with sigma of 0.01
 C16A, C15A, N7, O10A
 with sigma of 0.01
 C15, O10, N7A, C16
 with sigma of 0.01
 O16, C20, N6, C19
 with sigma of 0.01
 O20, C38, N5, C39, C47
 with sigma of 0.01
 O20A, C38A, N5A, C47A, C39A
 with sigma of 0.01
 O21A, C41A, N2A, C42A, C43A
 with sigma of 0.01
 O21, N2, C41, C42, C43
 with sigma of 0.01
 O21, C41, C43, C42, N2
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O16 \\sim N7A \\sim O10 \\sim N6 \\sim C15 \\sim C30 \\sim C16 \\sim C17 \\sim
C18 \\sim C19 \\sim C29 \\sim C20 \\sim O16A \\sim N7 \\sim O10A \\sim N6A
\\sim C15A \\sim C30A \\sim C16A \\sim C17A \\sim C18A \\sim C19A \\sim C29A
\\sim C20A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O20 \\sim N5 \\sim C39 \\sim C38 \\sim C47 \\sim O20A \\sim C38A \\sim N5A
\\sim C39A \\sim C47A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O21 \\sim N2 \\sim C41 \\sim C42 \\sim C43 \\sim O21A \\sim C41A \\sim N2A
\\sim C43A \\sim C42A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O22) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(N4)
\\sim Ueq, Uanis(C46) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O16) \\sim Ueq, Uanis(N7A) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(N6)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(O16A) \\sim Ueq, Uanis(N7) \\sim Ueq,
Uanis(O10A) \\sim Ueq, Uanis(N6A) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C30A)
\\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C18A) \\sim Ueq,
Uanis(C19A) \\sim Ueq, Uanis(C29A) \\sim Ueq, Uanis(C20A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(O20) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(O20A) \\sim Ueq, Uanis(C38A) \\sim Ueq,
Uanis(N5A) \\sim Ueq, Uanis(C39A) \\sim Ueq, Uanis(C47A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O21) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42)
\\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(O21A) \\sim Ueq, Uanis(C41A) \\sim Ueq,
Uanis(N2A) \\sim Ueq, Uanis(C43A) \\sim Ueq, Uanis(C42A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O16, N7A, O10, N6, C15, C30, C16, C17, C18, C19, C29, C20, O16A, N7, O10A,
 N6A, C15A, C30A, C16A, C17A, C18A, C19A, C29A, C20A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O20, N5, C39, C38, C47, O20A, C38A, N5A, C39A, C47A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O21, N2, C41, C42, C43, O21A, C41A, N2A, C43A, C42A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Sof(O16A)=Sof(N7)=Sof(H7B)=Sof(O10A)=Sof(N6A)=Sof(H6A)=Sof(C15A)=Sof(C30A)=
 Sof(H30A)=Sof(C16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=
 Sof(C29A)=Sof(H29A)=Sof(C20A)=1-FVAR(1)
 Sof(O16)=Sof(N7A)=Sof(H7A)=Sof(O10)=Sof(N6)=Sof(H6)=Sof(C15)=Sof(C30)=
 Sof(H30)=Sof(C16)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(C29)=
 Sof(H29)=Sof(C20)=FVAR(1)
 Sof(O21A)=Sof(C41A)=Sof(H41A)=Sof(N2A)=Sof(C43A)=Sof(H43D)=Sof(H43E)=
 Sof(H43F)=Sof(C42A)=Sof(H42D)=Sof(H42E)=Sof(H42F)=1-FVAR(2)
 Sof(O21)=Sof(N2)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(H42C)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(2)
 Sof(O20A)=Sof(C38A)=Sof(H38A)=Sof(N5A)=Sof(C39A)=Sof(H39D)=Sof(H39E)=
 Sof(H39F)=Sof(C47A)=Sof(H47D)=Sof(H47E)=Sof(H47F)=1-FVAR(3)
 Sof(O20)=Sof(N5)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C38)=Sof(H38)=
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=FVAR(3)
7.a Riding coordinates:
 C46(H46A,H46B,H46C), C42(H42A,H42B,H42C), C43A(H43D,H43E,H43F)
7.b Aromatic/amide H refined with riding coordinates:
 N7A(H7A), N3(H3), N6(H6), C3(H3A), C44(H44), C40(H40), C34(H34), C31(H31),
 C25(H25), C22(H22), C13(H13), C8(H8), C28(H28), C35(H35), C41(H41), C38(H38),
 C7(H7), C30(H30), C17(H17), C18(H18), C29(H29), N7(H7B), N6A(H6A), C30A(H30A),
 C17A(H17A), C18A(H18A), C29A(H29A), C41A(H41A), C38A(H38A), C0AA(H0AA)
7.c Fitted hexagon refined as free rotating group:
 C30(C16,C17,C18,C19,C29), C30A(C16A,C17A,C18A,C19A,C29A)
7.d Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C39(H39A,H39B,H39C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C43(H43A,H43B,H43C), C47(H47A,H47B,H47C), C42A(H42D,H42E,H42F),
 C39A(H39D,H39E,H39F), C47A(H47D,H47E,H47F)
;
_olex2_submission_special_instructions 'No special instructions were received'