Efficient synthetic route to heterobimetallic trinuclear complexes [Ln-Mn-Ln] and their single molecule magnetic properties
Filzah Ghazali, Nurul; Vignesh, Kuduva R.; Phonsri, Wasinee; Murray, Keith S.; Junk, Peter Courtney; Deacon, Glen B.; Turner, David Roger; Dalton Transactions  (2022) –; doi:10.1039/D2DT02616C

data_7711779
_publ_section_title
;
 Efficient synthetic route to heterobimetallic trinuclear complexes
 [Ln-Mn-Ln] and their single molecule magnetic properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02616C
_journal_year                    2022
_chemical_formula_moiety
'C36 H20 Cl4 Eu N4 O4, C16 H36 N, C2 H6 O, 2(H2 O)'
_chemical_formula_sum            'C54 H66 Cl4 Eu N5 O7'
_chemical_formula_weight         1190.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual-space
_audit_creation_date             2021-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-08-01 deposited with the CCDC.	2022-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.71(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.534(5)
_cell_length_b                   22.576(5)
_cell_length_c                   22.796(5)
_cell_measurement_reflns_used    371091
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.886
_cell_measurement_theta_min      0.949
_cell_volume                     11047(5)
_computing_cell_refinement       'XDS (Kansch, 1993)'
_computing_data_collection       'BluICE (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kansch, 1993)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  'double silicon'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            371091
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         31.886
_diffrn_reflns_theta_min         0.949
_diffrn_source                   'MX1 Beamline, Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.383
_exptl_absorpt_correction_T_max  'Not provided by XDS'
_exptl_absorpt_correction_T_min  'Not provided by XDS'
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       block
_exptl_crystal_F_000             4896
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
Elemental analysis suggets 4 x H2O and 2 x EtOH per void
Equates to 92 electrons per void, in close agreement
These solvents have been included in the chemical formula and UNIT
;
_refine_diff_density_max         2.431
_refine_diff_density_min         -2.217
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.00276(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1267
_refine_ls_number_reflns         31746
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0755P)^2^+9.4547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24723
_reflns_number_total             31746
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02616c2.cif
_cod_data_source_block           1Eu
_cod_database_code               7711779
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.934
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1C-C1A
 1.5 with sigma of 0.02
 C1A-C1C = C103-C102
 1.5 with sigma of 0.02
 C101-C102
 1.5 with sigma of 0.02
 C103-C102
 1.5 with sigma of 0.01
 C99-C98 \\sim C99A-C98
 with sigma of 0.02
3. Rigid bond restraints
 C99, C104
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C99A, C1D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C99 \\sim C104: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C99A \\sim C1D: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C1A)
\\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C1C) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C99A) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C1D) \\sim Ueq, Uanis(C99)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C1A, C1B, C1C, C100, C101, C102, C103
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1D, C98, C99, C99A, C104
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H82C)=Sof(H82D)=Sof(C83A)=Sof(H83C)=Sof(H83D)=Sof(C84A)=Sof(H84D)=
 Sof(H84E)=Sof(H84F)=1-FVAR(1)
 Sof(H82A)=Sof(H82B)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(C84)=Sof(H84A)=Sof(H84B)=
 Sof(H84C)=FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C1C)=Sof(H1CA)=
 Sof(H1CB)=Sof(H1CC)=Sof(H10C)=Sof(H10D)=1-FVAR(2)
 Sof(H10A)=Sof(H10B)=Sof(C101)=Sof(H10E)=Sof(H10F)=Sof(C102)=Sof(H10G)=
 Sof(H10H)=Sof(C103)=Sof(H10I)=Sof(H10J)=Sof(H10K)=FVAR(2)
 Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=Sof(H98C)=Sof(H98D)=Sof(C99A)=
 Sof(H99C)=Sof(H99D)=1-FVAR(3)
 Sof(H98A)=Sof(H98B)=Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(C104)=Sof(H10L)=
 Sof(H10M)=Sof(H10N)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,
 H75B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B), C81(H81A,H81B),
 C82(H82A,H82B), C82(H82C,H82D), C83(H83A,H83B), C83A(H83C,H83D), C85(H85A,
 H85B), C86(H86A,H86B), C87(H87A,H87B), C89(H89A,H89B), C90(H90A,H90B),
 C91(H91A,H91B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B), C97(H97A,H97B),
  C98(H98A,H98B), C98(H98C,H98D), C99(H99A,H99B), C99A(H99C,H99D), C100(H10A,
 H10B), C100(H10C,H10D), C101(H10E,H10F), C102(H10G,H10H)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27), C30(H30),
  C31(H31), C32(H32), C35(H35), C36(H36), C39(H39), C40(H40), C41(H41),
 C44(H44), C45(H45), C48(H48), C49(H49), C50(H50), C53(H53), C54(H54), C57(H57),
  C58(H58), C59(H59), C62(H62), C63(H63), C66(H66), C67(H67), C68(H68),
 C71(H71), C72(H72)
7.c Idealised Me refined as rotating group:
 C1C(H1CA,H1CB,H1CC), C1D(H1DA,H1DB,H1DC), C76(H76A,H76B,H76C), C80(H80A,H80B,
 H80C), C84(H84A,H84B,H84C), C84A(H84D,H84E,H84F), C88(H88A,H88B,H88C),
 C92(H92A,H92B,H92C), C96(H96A,H96B,H96C), C103(H10I,H10J,H10K), C104(H10L,H10M,
 H10N)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              78924
_shelx_hkl_checksum              79843
_shelx_fab_checksum              94769
_olex2_submission_special_instructions 'No special instructions were received'