Complementation and joint contribution of appropriate intramolecular coupling and local ion symmetry to improve magnetic relaxation in a series of dinuclear Dy2 single-molecule magnets
Tu, Hao-Ran; Sun, Wen-Bin; Li, Hong-Feng; Chen, Peng; Tian, Yong-Mei; Zhang, Wan-Ying; Zhang, Yi-Quan; Yan, Peng-Fei; Inorganic Chemistry Frontiers 4 (2017) 499–; doi:10.1039/C6QI00508J

data_4349628
_publ_section_title
;
 Complementation and joint contribution of appropriate intramolecular
 coupling and local ion symmetry to improve magnetic relaxation in a
 series of dinuclear Dy2 single-molecule magnets
;
_journal_issue                   3
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              499
_journal_paper_doi               10.1039/C6QI00508J
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         'C72 H50 Er2 F12 O14'
_chemical_formula_sum            'C72 H50 Er2 F12 O14'
_chemical_formula_weight         1701.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-01-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-03-10 deposited with the CCDC.
2016-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.158(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.1533(5)
_cell_length_b                   14.2224(3)
_cell_length_c                   18.6514(5)
_cell_measurement_reflns_used    5561
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6875
_cell_measurement_theta_min      3.0980
_cell_volume                     6696.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.875
_diffrn_measurement_details
;
  1 omega   59.00  108.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4268  178.0000   90.0000 49

  2 omega  -60.00   49.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6768   77.0000  -90.0000 109

  3 omega  -10.00   16.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6768  -99.0000  -30.0000 26

  4 omega  -47.00   54.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6768    0.0000 -120.0000 101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0115500000
_diffrn_orient_matrix_UB_12      0.0213799000
_diffrn_orient_matrix_UB_13      0.0348399000
_diffrn_orient_matrix_UB_21      0.0054129000
_diffrn_orient_matrix_UB_22      -0.0450537000
_diffrn_orient_matrix_UB_23      0.0165581000
_diffrn_orient_matrix_UB_31      0.0250385000
_diffrn_orient_matrix_UB_32      -0.0001112000
_diffrn_orient_matrix_UB_33      -0.0080566000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17264
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.75
_diffrn_reflns_theta_min         3.10
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    2.588
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3352
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         8364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+15.5390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.1054
_reflns_number_gt                5857
_reflns_number_total             8364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00508j4.cif
_cod_data_source_block           exp_11161
_cod_database_code               4349628
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(F0AB)=Sof(F1A)=Sof(F3A)=1-FVAR(1)
 Sof(F4)=Sof(F6)=Sof(F5)=FVAR(1)
 Sof(C3AB)=Sof(H3AB)=Sof(C1AB)=Sof(C2AB)=Sof(H2AB)=Sof(C5A)=Sof(H5A)=Sof(C4AB)=
 Sof(C4A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C6A)=Sof(H6A)=Sof(C3A)=
 Sof(H3A)=1-FVAR(2)
 Sof(C9)=Sof(C8)=Sof(H8)=Sof(C10)=Sof(H10)=Sof(C5)=Sof(C7)=Sof(H7)=Sof(C6)=
 Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C4)=Sof(H4)=Sof(C3)=Sof(H3)=FVAR(2)
3.a Aromatic/amide H refined with riding coordinates:
 C34(H34), C22(H22), C26(H26), C12(H12), C33(H33), C21(H21), C24(H24),
 C32(H32), C17(H17), C18(H18), C15(H15), C16(H16), C8(H8), C10(H10), C7(H7),
 C1(H1), C2(H2), C4(H4), C3(H3), C3AB(H3AB), C2AB(H2AB), C5A(H5A), C1A(H1A),
 C2A(H2A), C6A(H6A), C3A(H3A)
3.b Idealised Me refined as rotating group:
 C36(H36a,H36b,H36c), C29(H29a,H29b,H29c)
;
_olex2_submission_special_instructions 'No special instructions were received'