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_7240317
_publ_section_title
;
 The different magnetic relaxation behaviors in [Fe(CN)6]3&#x2212; or
 [Co(CN)6]3&#x2212; bridged 3d--4f heterometallic compounds
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00039F
_journal_year                    2020
_chemical_formula_moiety         'C60 H56 Dy2 Fe2 N28 O8, 5(H2 O)'
_chemical_formula_sum            'C60 H66 Dy2 Fe2 N28 O13'
_chemical_formula_weight         1824.10
_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     iterative
_audit_creation_date             2019-12-30
_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                78.099(5)
_cell_angle_beta                 87.212(5)
_cell_angle_gamma                70.357(6)
_cell_formula_units_Z            1
_cell_length_a                   11.7703(8)
_cell_length_b                   12.8448(8)
_cell_length_c                   12.8648(7)
_cell_measurement_reflns_used    5493
_cell_measurement_temperature    122.65(10)
_cell_measurement_theta_max      28.5430
_cell_measurement_theta_min      3.3110
_cell_volume                     1792.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      122.65(10)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -16.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497   19.0000 -120.0000 102

  2 omega   25.00   60.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497  -99.0000 -180.0000 35

  3 omega  -51.00   45.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497  -77.0000  -60.0000 96

  4 omega  -12.00   84.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497   77.0000   60.0000 96

  5 omega  -45.00    9.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5841   77.0000 -120.0000 54
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0516279000
_diffrn_orient_matrix_UB_12      -0.0493563000
_diffrn_orient_matrix_UB_13      0.0105363000
_diffrn_orient_matrix_UB_21      0.0375520000
_diffrn_orient_matrix_UB_22      0.0338755000
_diffrn_orient_matrix_UB_23      -0.0056611000
_diffrn_orient_matrix_UB_31      -0.0045472000
_diffrn_orient_matrix_UB_32      0.0005591000
_diffrn_orient_matrix_UB_33      0.0550762000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12022
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.906
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.538
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.690
_exptl_crystal_description       block
_exptl_crystal_F_000             910
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.388
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6290
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0338P)^2^+1.8121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5568
_reflns_number_total             6290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00039f2.cif
_cod_data_source_block           p150401e
_cod_database_code               7240317
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1O1N1DY1FE1
_chemical_oxdiff_usercomment     2015032701
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: O5(0.5) H5A(0.5) H5B(0.5)
4.a Riding coordinates:
 O4(H4A,H4B), O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N7(H7), C1(H1), C2(H2A), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12),
  C18(H18), C19(H19), C20(H20), C21(H21), C28(H28)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              50618
_olex2_submission_special_instructions 'No special instructions were received'