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_7711772
_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
'C72 H40 Cl8 Mn N8 O8 Tb2, 2(C0.75 H0.75 Cl2.25)'
_chemical_formula_sum            'C73.5 H41.5 Cl12.5 Mn N8 O8 Tb2'
_chemical_formula_weight         1980.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                101.43(3)
_cell_angle_beta                 109.82(3)
_cell_angle_gamma                99.23(3)
_cell_formula_units_Z            1
_cell_length_a                   12.134(2)
_cell_length_b                   12.569(3)
_cell_length_c                   13.561(3)
_cell_measurement_reflns_used    7306
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     1848.1(9)
_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(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.967
_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  0.0548
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            37092
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.244
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.659
_diffrn_source                   'MX1 Beamline, Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.575
_exptl_absorpt_correction_T_max  'not provided by XDS'
_exptl_absorpt_correction_T_min  'not provided by XDS'
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS(Kabsch, 1993)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             970
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.609
_refine_diff_density_min         -1.358
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         7306
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+3.8548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6892
_reflns_number_total             7306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02616c2.cif
_cod_data_source_block           2Tb
_cod_original_cell_volume        1848.1(8)
_cod_original_formula_sum        'C73.50 H41.50 Cl12.50 Mn N8 O8 Tb2'
_cod_database_code               7711772
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.627
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl6A-C37 \\sim Cl6B-C37 \\sim Cl7A-C37 \\sim Cl7B-C37 \\sim Cl5-C37
 with sigma of 0.02
3. Others
 Fixed Sof: Cl5(0.75) Cl6A(0.5) Cl6B(0.25) Cl7A(0.5) Cl7B(0.25) C37(0.75)
 H37A(0.25) H37(0.5)
4.a Ternary CH refined with riding coordinates:
 C37(H37A), C37(H37)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C28(H28),
  C29(H29), C30(H30), C33(H33), C34(H34)
;
_shelx_res_checksum              9318
_shelx_hkl_checksum              2672
_olex2_submission_special_instructions 'No special instructions were received'