Magnetic hysteresis in 1D organometallic lanthanide chain compounds containing 4,4'-bipyridine.
Castellanos, Ernesto; Benner, Florian; Deshapriya, Saroshan; Demir, Selvan; Chemical science 16 (2025) 18616–18631; doi:10.1039/d5sc05460e

data_1575901
_publ_section_title
;
 Magnetic hysteresis in 1D organometallic lanthanide chain compounds
 containing 4,4'-bipyridine.
;
_journal_issue                   40
_journal_name_full               'Chemical science'
_journal_page_first              18616
_journal_page_last               18631
_journal_paper_doi               10.1039/d5sc05460e
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety
'C30 H38 Gd N2, C24 H20 B, 3(C2 H4 O0.50), 2(C2 H4 O0.50)'
_chemical_formula_sum            'C66 H82 B Gd N2 O3'
_chemical_formula_weight         1119.39
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-16
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2025-07-21 deposited with the CCDC.	2025-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.353(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4145(8)
_cell_length_b                   21.4824(5)
_cell_length_c                   17.5221(7)
_cell_measurement_reflns_used    12191
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.2290
_cell_measurement_theta_min      2.3090
_cell_volume                     5713.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33311
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.825
_diffrn_reflns_theta_min         2.496
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.208
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.359
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       block
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.148
_refine_diff_density_max         3.055
_refine_diff_density_min         -2.071
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         6731
_refine_ls_number_restraints     721
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0556P)^2^+38.1001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5573
_reflns_number_total             6731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05460e2.cif
_cod_data_source_block           ec-1-94gd-xprepc2c
_cod_depositor_comments
'Adding full bibliography for 1575900--1575902.cif.'
_cod_original_cell_volume        5713.6(5)
_cod_database_code               1575901
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.743
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3-C2 = C3-C4 = C2-C1 = C1-C5 = C5-C4
 1.42 with sigma of 0.02
 C3-C8 = C4-C9
 1.5 with sigma of 0.02
 C2-C7 = C1-C6 = C5-C10
 1.51 with sigma of 0.02
 C15-C11 = C15-C14 = C11-C12 = C12-C13 = C13-C14
 1.42 with sigma of 0.02
 C15-C20 = C14-C19
 1.5 with sigma of 0.02
 C11-C16 = C12-C17 = C13-C18
 1.51 with sigma of 0.02
 C5S-O2 = C5S-C6S
 1.44 with sigma of 0.02
 O2-C8S = C7S-C6S
 1.53 with sigma of 0.02
 C8S-C7S
 1.54 with sigma of 0.02
 C2S-C3S
 1.54 with sigma of 0.02
 O1-C1S = O1-C4S
 1.44 with sigma of 0.02
 C1S-C2S = C3S-C4S
 1.53 with sigma of 0.02
 C12S-C11S = C10S-C9S
 1.53 with sigma of 0.02
 O3-C12S = O3-C9S
 1.44 with sigma of 0.02
 C11S-C10S
 1.54 with sigma of 0.02
 C1A-C1B = C1D-C1E
 1.38 with sigma of 0.02
 C3-C7 = C3-C9 = C2-C6
 2.6 with sigma of 0.04
 C3-C1 = C3-C5
 2.29 with sigma of 0.04
 C1-C10 = C5-C9
 2.61 with sigma of 0.04
 C2-C5 = C1-C4
 2.3 with sigma of 0.04
 C11-C13 = C12-C14
 2.3 with sigma of 0.04
 C15-C12 = C15-C13
 2.29 with sigma of 0.04
 C15-C16 = C15-C19 = C11-C17
 2.6 with sigma of 0.04
 C12-C18 = C13-C19
 2.61 with sigma of 0.04
 C5S-C8S = C5S-C7S = O2-C7S = C8S-C6S
 2.38 with sigma of 0.04
 O1-C2S = O1-C3S = C1S-C3S = C2S-C4S
 2.38 with sigma of 0.04
 O3-C11S = O3-C10S = C12S-C10S = C11S-C9S
 2.38 with sigma of 0.04
 C1B-C1D
 2.35 with sigma of 0.04
 C8-C2 \\sim C8-C4 \\sim C7-C3 \\sim C7-C1 \\sim C6-C2 \\sim C6-C5 \\sim C10-C1
\\sim C10-C4 \\sim C9-C5 \\sim C9-C3
 with sigma of 0.04
 C3-C8 \\sim C2-C7 \\sim C1-C6 \\sim C5-C10 \\sim C4-C9
 with sigma of 0.02
 C3-C2 \\sim C2-C1 \\sim C1-C5 \\sim C5-C4 \\sim C4-C3
 with sigma of 0.02
 C3-C1 \\sim C2-C5 \\sim C1-C4 \\sim C4-C2 \\sim C3-C5
 with sigma of 0.04
 C15-C20 \\sim C11-C16 \\sim C12-C17 \\sim C13-C18 \\sim C14-C19
 with sigma of 0.02
 C20-C11 \\sim C20-C14 \\sim C16-C15 \\sim C16-C12 \\sim C17-C11 \\sim C17-C13
\\sim C18-C12 \\sim C18-C14
 \\sim C19-C13 \\sim C19-C15
 with sigma of 0.04
 C15-C11 \\sim C11-C12 \\sim C12-C13 \\sim C13-C14 \\sim C14-C15
 with sigma of 0.02
 C15-C12 \\sim C11-C13 \\sim C12-C14 \\sim C14-C11 \\sim C15-C13
 with sigma of 0.04
 C8S-C6S \\sim O2-C7S
 with sigma of 0.04
 C5S-C8S \\sim C5S-C7S
 with sigma of 0.04
 O2-C8S \\sim C8S-C7S \\sim C7S-C6S
 with sigma of 0.02
 C5S-O2 \\sim C5S-C6S
 with sigma of 0.02
 C1S-C2S \\sim C2S-C3S \\sim C3S-C4S
 with sigma of 0.02
 O1-C1S \\sim O1-C4S
 with sigma of 0.02
 O1-C2S \\sim O1-C3S
 with sigma of 0.04
 C2S-C4S \\sim C1S-C3S
 with sigma of 0.04
 C12S-C11S \\sim C11S-C10S \\sim C10S-C9S
 with sigma of 0.02
 O3-C12S \\sim O3-C9S
 with sigma of 0.02
 C11S-C9S \\sim C12S-C10S
 with sigma of 0.04
 O3-C11S \\sim O3-C10S
 with sigma of 0.04
 C1D-C1B \\sim C1E-C1A
 with sigma of 0.04
 C1A-C1B \\sim C1D-C1E
 with sigma of 0.02
3. Restrained planarity
 C3, C2, C1, C5, C4, C9, C10, C6, C7, C8
 with sigma of 0.1
 C15, C11, C12, C13, C14, C19, C18, C17, C16, C20
 with sigma of 0.1
 C1A, C1B, C1D, C1E
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C3 \\sim C2 \\sim C1 \\sim C5 \\sim C4 \\sim C9 \\sim C10 \\sim C6 \\sim C7
\\sim C8: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C15 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C19 \\sim C18 \\sim C17 \\sim
C16 \\sim C20: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C5S \\sim O2 \\sim C8S \\sim C7S \\sim C6S: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O1 \\sim C1S \\sim C2S \\sim C3S \\sim C4S: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O3 \\sim C12S \\sim C11S \\sim C10S \\sim C9S: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C1A \\sim C1B \\sim C1D \\sim C1E: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(C3) = Uanis(C11)
Uanis(C14) = Uanis(C5)
Uanis(C9) = Uanis(C20)
Uanis(C19) = Uanis(C10)
Uanis(C7) = Uanis(C17)
Uanis(C13) = Uanis(C1)
Uanis(C18) = Uanis(C6)
Uanis(C4) = Uanis(C15)
Uanis(C2) = Uanis(C12)
Uanis(C8) = Uanis(C16)
Uanis(C5S) = Uanis(O1)
5. Rigid body (RIGU) restrains
 C3, C2, C1, C5, C4, C9, C10, C6, C7, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15, C11, C12, C13, C14, C19, C18, C17, C16, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5S, O2, C8S, C7S, C6S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C1S, C2S, C3S, C4S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C12S, C11S, C10S, C9S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1A, C1B, C1D, C1E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C1(0.5) C2(0.5) C3(0.5) C4(0.5) C5(0.5) C6(0.5) H6A(0.5) H6B(0.5)
 H6C(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5)
 C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5) C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
 C11(0.5) C12(0.5) C13(0.5) C14(0.5) C15(0.5) C16(0.5) H16A(0.5) H16B(0.5)
 H16C(0.5) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C18(0.5) H18A(0.5) H18B(0.5)
 H18C(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C20(0.5) H20A(0.5) H20B(0.5)
 H20C(0.5) O1(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5)
 C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) O3(0.5) C9S(0.5)
 H9SA(0.5) H9SB(0.5) C10S(0.5) H10D(0.5) H10E(0.5) C11S(0.5) H11A(0.5)
 H11B(0.5) C12S(0.5) H12A(0.5) H12B(0.5) C7S(0.5) H7SA(0.5) H7SB(0.5) O2(0.5)
 C5S(0.5) H5SA(0.5) H5SB(0.5) C6S(0.5) H6SA(0.5) H6SB(0.5) C8S(0.5) H8SA(0.5)
 H8SB(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C9S(H9SA,
 H9SB), C10S(H10D,H10E), C11S(H11A,H11B), C12S(H12A,H12B), C7S(H7SA,H7SB),
 C5S(H5SA,H5SB), C6S(H6SA,H6SB), C8S(H8SA,H8SB)
7.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C1B(H1B), C1D(H1D), C1E(H1E), C27(H27), C28(H28), C29(H29),
 C30(H30), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37)
7.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              28720
_olex2_submission_special_instructions 'No special instructions were received'