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_7711775
_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 N4 O4 Yb, C16 H36 N, 2(C2 H6 O)'
_chemical_formula_sum            'C56 H68 Cl4 N5 O6 Yb'
_chemical_formula_weight         1221.99
_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                 107.68(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.672(5)
_cell_length_b                   22.311(5)
_cell_length_c                   22.597(5)
_cell_measurement_reflns_used    2167
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     10890(5)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.953
_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  0.0767
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            162583
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.244
_diffrn_reflns_theta_max         27.514
_diffrn_reflns_theta_min         0.943
_diffrn_source                   'MX1 Beamline, Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.968
_exptl_absorpt_correction_T_max  'Not supplied by XDS'
_exptl_absorpt_correction_T_min  'Not supplied by XDS'
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5000
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.156
_refine_diff_density_min         -3.051
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1228
_refine_ls_number_reflns         23873
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0736
_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^)+(0.0558P)^2^+124.8607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1835
_refine_ls_wR_factor_ref         0.1974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17266
_reflns_number_total             23873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02616c2.cif
_cod_data_source_block           yb_sq
_cod_database_code               7711775
_shelx_shelxl_version_number     2018/3
_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
 C82-C81 = C81-C82A
 1.5 with sigma of 0.02
 C91-C90
 1.5 with sigma of 0.02
 C102-C103
 1.5 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C80, C81, C82, C83, C88, C89, C90, C91, C100, C101, C102, C103
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1A, C101, C102, C103
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H81C)=Sof(H81D)=Sof(C82A)=Sof(H82C)=Sof(H82D)=Sof(C83A)=Sof(H83D)=
 Sof(H83E)=Sof(H83F)=1-FVAR(1)
 Sof(H81A)=Sof(H81B)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(C83)=Sof(H83A)=Sof(H83B)=
 Sof(H83C)=FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(H10G)=Sof(H10H)=1-FVAR(2)
 Sof(H10E)=Sof(H10F)=Sof(C103)=Sof(H10I)=Sof(H10J)=Sof(H10K)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C76(H76A,H76B), C77(H77A,
 H77B), C78(H78A,H78B), C80(H80A,H80B), C81(H81A,H81B), C81(H81C,H81D),
 C82(H82A,H82B), C82A(H82C,H82D), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,
 H86B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B), C92(H92A,H92B),
 C93(H93A,H93B), C94(H94A,H94B), C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B),
  C100(H10A,H10B), C101(H10C,H10D), C102(H10E,H10F), C102(H10G,H10H)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C29(H29),
  C30(H30), C31(H31), C34(H34), C35(H35), C38(H38), C39(H39), C42(H42),
 C43(H43), C44(H44), C47(H47), C48(H48), C49(H49), C52(H52), C53(H53), C56(H56),
  C57(H57), C58(H58), C61(H61), C62(H62), C65(H65), C66(H66), C69(H69),
 C70(H70), C71(H71)
5.c Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C75(H75A,H75B,H75C), C79(H79A,H79B,H79C), C83(H83A,H83B,
 H83C), C83A(H83D,H83E,H83F), C87(H87A,H87B,H87C), C91(H91A,H91B,H91C),
 C95(H95A,H95B,H95C), C99(H99A,H99B,H99C), C103(H10I,H10J,H10K)
;
_shelx_res_checksum              11407
_shelx_hkl_checksum              45093
_shelx_fab_checksum              86001
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'