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_7711776
_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 Dy N4 O4, C16 H36 N, C2 H6 O, 2(H2 O)'
_chemical_formula_sum            'C54 H66 Cl4 Dy N5 O7'
_chemical_formula_weight         1201.41
_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             2022-03-03
_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                 107.79(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.599(5)
_cell_length_b                   22.428(5)
_cell_length_c                   22.699(5)
_cell_measurement_reflns_used    19097
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      0.946
_cell_volume                     10955(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(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.1058
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            128046
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         0.946
_diffrn_source                   'MX1 Beamline, Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.614
_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    1.457
_exptl_crystal_description       block
_exptl_crystal_F_000             4920
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.100
_refine_diff_density_min         -1.820
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1266
_refine_ls_number_reflns         19097
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+74.9778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13885
_reflns_number_total             19097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02616c2.cif
_cod_data_source_block           dy_sq
_cod_database_code               7711776
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.924
_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
 C83-C82 = C82-C83A
 1.5 with sigma of 0.02
 C99A-C98A
 1.5 with sigma of 0.02
 C100-C98
 2.5 with sigma of 0.02
 C98A-C99A = C99A-C1C
 1.5 with sigma of 0.02
 C1A-C1B
 1.5 with sigma of 0.02
 H93B-H98A
 2.2 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C103, C104, C1A, C1B, C102
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C97, C98, C99, C100, C99A, C1C, C98A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. 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(H10H)=Sof(H10I)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1B)=Sof(H1BA)=
 Sof(H1BB)=1-FVAR(2)
 Sof(H10F)=Sof(H10G)=Sof(C103)=Sof(H10J)=Sof(H10K)=Sof(C104)=Sof(H10L)=
 Sof(H10M)=Sof(H10N)=FVAR(2)
 Sof(H97C)=Sof(H97D)=Sof(C99A)=Sof(H99C)=Sof(H99D)=Sof(C1C)=Sof(H1CA)=
 Sof(H1CB)=Sof(H1CC)=Sof(C98A)=Sof(H98C)=Sof(H98D)=1-FVAR(3)
 Sof(H97A)=Sof(H97B)=Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(C99)=Sof(H99A)=Sof(H99B)=
 Sof(C100)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 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), 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), C97(H97C,H97D), C98(H98A,H98B), C99(H99A,H99B),
 C101(H10D,H10E), C102(H10H,H10I), C102(H10F,H10G), C103(H10J,H10K), C83A(H83C,
 H83D), C1B(H1BA,H1BB), C99A(H99C,H99D), C98A(H98C,H98D)
5.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)
5.c Idealised Me refined as rotating group:
 C76(H76A,H76B,H76C), C80(H80A,H80B,H80C), C84(H84A,H84B,H84C), C88(H88A,H88B,
 H88C), C92(H92A,H92B,H92C), C96(H96A,H96B,H96C), C100(H10A,H10B,H10C),
 C104(H10L,H10M,H10N), C84A(H84D,H84E,H84F), C1A(H1AA,H1AB,H1AC), C1C(H1CA,H1CB,
 H1CC)
;
_shelx_res_checksum              4304
_shelx_hkl_checksum              86369
_shelx_fab_checksum              82212
_olex2_submission_special_instructions 'No special instructions were received'