The different magnetic relaxation behaviors in [Fe(CN)6]3− or [Co(CN)6]3− bridged 3d‒4f heterometallic compounds
Wang, Ruirui; Wang, Haili; Wang, Juan; Bai, Feifei; Ma, Yue; Li, Licun; Wang, Qinglun; Zhao, Bin; Cheng, Peng; CrystEngComm  (2020) –; doi:10.1039/D0CE00039F

data_7240314
_publ_section_title
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 The different magnetic relaxation behaviors in [Fe(CN)6]3&#x2212; or
 [Co(CN)6]3&#x2212; bridged 3d--4f heterometallic compounds
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00039F
_journal_year                    2020
_chemical_formula_moiety         'C60 H56 Fe2 N28 O8 Tb2, 5(H2 O)'
_chemical_formula_sum            'C60 H66 Fe2 N28 O13 Tb2'
_chemical_formula_weight         1816.94
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-01-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-06 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                77.643(3)
_cell_angle_beta                 87.270(3)
_cell_angle_gamma                70.613(3)
_cell_formula_units_Z            1
_cell_length_a                   11.8312(10)
_cell_length_b                   12.9358(11)
_cell_length_c                   12.9377(11)
_cell_measurement_reflns_used    9093
_cell_measurement_temperature    297.0
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      3.10
_cell_volume                     1823.9(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      297.0
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0891
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            60304
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.315
_diffrn_reflns_theta_min         3.098
_exptl_absorpt_coefficient_mu    2.384
_exptl_absorpt_correction_T_max  0.7945
_exptl_absorpt_correction_T_min  0.3066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'metallic orangish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_description       block
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.376
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         6560
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0537
_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^)+19.4382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1073
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5578
_reflns_number_total             6560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00039f2.cif
_cod_data_source_block           20150527c_0m
_cod_database_code               7240314
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.647
_shelx_estimated_absorpt_t_min   0.647
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H6a-N13_$1
 2 with sigma of 0.02
 H1-H16c
 2.2 with sigma of 0.02
 H4a-O4 = O4-H4b
 0.85 with sigma of 0.02
3. Others
 Fixed Sof: O5(0.5) H5a(0.5) H5b(0.5)
4.a Riding coordinates:
 O4(H4a,H4b), O5(H5a,H5b), O7(H7a,H7b)
4.b Free rotating group:
 O6(H6a,H6b)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14),
 C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22)
4.d Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C16(H16a,H16b,H16c), C23(H23a,H23b,H23c), C24(H24a,H24b,
 H24c)
;
_shelx_res_checksum              41699
_olex2_submission_special_instructions 'No special instructions were received'