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_7711778
_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 Ho N4 O4, C16 H36 N, 3(H2 O), C2 H6 O'
_chemical_formula_sum            'C54 H68 Cl4 Ho N5 O8'
_chemical_formula_weight         1221.86
_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                 107.882(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.4676(3)
_cell_length_b                   22.5189(2)
_cell_length_c                   22.7200(3)
_cell_measurement_reflns_used    66900
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      33.5820
_cell_measurement_theta_min      2.5220
_cell_volume                     10939.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     33.00  74.00   0.50   11.79    --   11.86  38.00 -90.00   82
  2  \w    -10.00  47.00   0.50   11.79    --   11.86-103.00   8.00  114
  3  \w     39.00  84.00   0.50   11.79    --   11.86 178.00 -60.00   90
  4  \w     39.00  84.00   0.50   11.79    --   11.86 178.00  30.00   90
  5  \w     -3.00  84.00   0.50   11.79    --   11.86  57.00 150.00  174
  6  \w    -20.00  21.00   0.50   11.79    --  -12.95 -99.00  90.00   82
  7  \w     36.00  84.00   0.50   11.79    --   11.86-178.00  90.00   96
  8  \w    -61.00  24.00   0.50   11.79    --   11.86 -38.00  90.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0061327000
_diffrn_orient_matrix_UB_12      0.0155611000
_diffrn_orient_matrix_UB_13      0.0246460000
_diffrn_orient_matrix_UB_21      -0.0070366000
_diffrn_orient_matrix_UB_22      0.0259512000
_diffrn_orient_matrix_UB_23      -0.0185334000
_diffrn_orient_matrix_UB_31      -0.0318534000
_diffrn_orient_matrix_UB_32      -0.0087295000
_diffrn_orient_matrix_UB_33      -0.0111562000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            176620
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.544
_diffrn_reflns_theta_min         2.407
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.699
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       block
_exptl_crystal_F_000             5008
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.561
_refine_diff_density_min         -1.633
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1257
_refine_ls_number_reflns         38081
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0334P)^2^+0.2744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0823
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28000
_reflns_number_total             38081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02616c2.cif
_cod_data_source_block           1Ho
_cod_database_code               7711778
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         HoCHNOCl
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_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
 C88-C87 = C87-C88A
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1C) \\sim Ueq, Uanis(C93A) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C92)
\\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq,
Uanis(C1B) \\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C92, C93, C93A, C103, C104, C105, C1A, C1B, C1C, C102
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H87C)=Sof(H87D)=Sof(C88A)=Sof(H88C)=Sof(H88D)=Sof(C89A)=Sof(H89D)=
 Sof(H89E)=Sof(H89F)=1-FVAR(1)
 Sof(H87A)=Sof(H87B)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(C89)=Sof(H89A)=Sof(H89B)=
 Sof(H89C)=FVAR(1)
 Sof(H92C)=Sof(H92D)=Sof(C93A)=Sof(H93D)=Sof(H93E)=Sof(H93F)=1-FVAR(2)
 Sof(H92A)=Sof(H92B)=Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=FVAR(2)
 Sof(H10H)=Sof(H10I)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=
 Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=1-FVAR(3)
 Sof(H10F)=Sof(H10G)=Sof(C103)=Sof(H10J)=Sof(H10K)=Sof(C104)=Sof(H10L)=
 Sof(H10M)=Sof(C105)=Sof(H10N)=Sof(H10O)=Sof(H10P)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C78(H78A,H78B), C79(H79A,
 H79B), C80(H80A,H80B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B),
 C86(H86A,H86B), C87(H87A,H87B), C87(H87C,H87D), C88(H88A,H88B), C90(H90A,H90B),
  C91(H91A,H91B), C92(H92A,H92B), C92(H92C,H92D), C94(H94A,H94B), C95(H95A,
 H95B), C96(H96A,H96B), C98(H98A,H98B), C99(H99A,H99B), C100(H10A,H10B),
 C102(H10F,H10G), C102(H10H,H10I), C103(H10J,H10K), C104(H10L,H10M), C88A(H88C,
 H88D), C1A(H1AA,H1AB), C1B(H1BA,H1BB)
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), C67(H67), C68(H68), C69(H69),
 C72(H72), C73(H73)
6.c Idealised Me refined as rotating group:
 C77(H77A,H77B,H77C), C81(H81A,H81B,H81C), C85(H85A,H85B,H85C), C89(H89A,H89B,
 H89C), C93(H93A,H93B,H93C), C97(H97A,H97B,H97C), C101(H10C,H10D,H10E),
 C105(H10N,H10O,H10P), C89A(H89D,H89E,H89F), C93A(H93D,H93E,H93F), C1C(H1CA,
 H1CB,H1CC)
;
_shelx_res_checksum              96435
_shelx_hkl_checksum              19716
_shelx_fab_checksum              35557
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.047
_oxdiff_exptl_absorpt_empirical_full_min 0.266