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_7711777
_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 Er N4 O4, C16 H36 NC16 H36 N, 3(H2 O), C2 H6 O'
_chemical_formula_sum            'C54 H68 Cl4 Er N5 O8'
_chemical_formula_weight         1224.19
_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
_audit_creation_date             2022-06-08
_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                 107.66(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.593(5)
_cell_length_b                   22.512(5)
_cell_length_c                   22.757(5)
_cell_measurement_reflns_used    2098
_cell_measurement_temperature    123.0
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     11029(5)
_computing_cell_refinement       Saint
_computing_data_collection       Saint
_computing_data_reduction        Saint
_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      123.0
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_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       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            126454
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         0.946
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.772
_exptl_absorpt_correction_T_max  0.3015
_exptl_absorpt_correction_T_min  0.1776
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       prism
_exptl_crystal_F_000             5016
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.056
_refine_diff_density_min         -2.110
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1266
_refine_ls_number_reflns         19172
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+10.7711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1138
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18037
_reflns_number_total             19172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02616c2.cif
_cod_data_source_block           1Er
_cod_database_code               7711777
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.843
_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
 C81A-C80 = C80-C81
 1.5 with sigma of 0.02
 C97A-C96 = C96-C97
 1.5 with sigma of 0.02
 C98A-C97A = C98-C97
 1.5 with sigma of 0.02
 C98A-C96
 2.5 with sigma of 0.02
 C102-C101
 1.5 with sigma of 0.02
 C101-C100
 1.5 with sigma of 0.02
 C1B-C100 = C100-C101
 1.5 with sigma of 0.01
 C102-C101 = C1B-C1A
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C102) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1B) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C1A)
\\sim Ueq, Uanis(C100) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C96) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C98A) \\sim Ueq, Uanis(C98)
\\sim Ueq, Uanis(C97A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C96) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C80, C81, C82, C81A, C82A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C96, C97A, C97, C98A, C98
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C102, C101, C100, C99
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C100, C101, C1A, C1B, C102
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C96, C95
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H80C)=Sof(H80D)=Sof(C81A)=Sof(H81C)=Sof(H81D)=Sof(C82A)=Sof(H82D)=
 Sof(H82E)=Sof(H82F)=1-FVAR(1)
 Sof(H80A)=Sof(H80B)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(C82)=Sof(H82A)=Sof(H82B)=
 Sof(H82C)=FVAR(1)
 Sof(H95C)=Sof(H95D)=Sof(C97A)=Sof(H97C)=Sof(H97D)=Sof(C98A)=Sof(H98D)=
 Sof(H98E)=Sof(H98F)=Sof(C96A)=Sof(H96C)=Sof(H96D)=1-FVAR(2)
 Sof(H95A)=Sof(H95B)=Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(C97)=Sof(H97A)=Sof(H97B)=
 Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(H98C)=FVAR(2)
 Sof(H10C)=Sof(H10D)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1B)=Sof(H1BA)=
 Sof(H1BB)=1-FVAR(3)
 Sof(H10A)=Sof(H10B)=Sof(C101)=Sof(H10E)=Sof(H10F)=Sof(C102)=Sof(H10G)=
 Sof(H10H)=Sof(H10I)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B), C79(H79A,H79B), C80(H80A,
 H80B), C80(H80C,H80D), C81(H81A,H81B), C83(H83A,H83B), C84(H84A,H84B),
 C85(H85A,H85B), C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B), C91(H91A,H91B),
  C92(H92A,H92B), C93(H93A,H93B), C95(H95A,H95B), C95(H95C,H95D), C96(H96A,
 H96B), C97(H97A,H97B), C99(H99A,H99B), C100(H10A,H10B), C100(H10C,H10D),
 C101(H10E,H10F), C103(H10J,H10K), C104(H10L,H10M), C105(H10N,H10O), C81A(H81C,
 H81D), C97A(H97C,H97D), C1B(H1BA,H1BB), C96A(H96C,H96D)
6.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)
6.c Idealised Me refined as rotating group:
 C78(H78A,H78B,H78C), C82(H82A,H82B,H82C), C86(H86A,H86B,H86C), C90(H90A,H90B,
 H90C), C94(H94A,H94B,H94C), C98(H98A,H98B,H98C), C102(H10G,H10H,H10I),
 C106(H10P,H10Q,H10R), C82A(H82D,H82E,H82F), C98A(H98D,H98E,H98F), C1A(H1AA,
 H1AB,H1AC)
;
_shelx_res_checksum              98745
_shelx_hkl_checksum              24262
_shelx_fab_checksum              97943
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'