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_4349634
_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 Dy2 F12 O14'
_chemical_formula_sum            'C72 H50 Dy2 F12 O14'
_chemical_formula_weight         1692.17
_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'
_symmetry_Int_Tables_number      15
_audit_creation_date             2015-04-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-09 deposited with the CCDC.
2016-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.255(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.2297(6)
_cell_length_b                   14.2596(3)
_cell_length_c                   18.5801(5)
_cell_measurement_reflns_used    6177
_cell_measurement_theta_max      30.0775
_cell_measurement_theta_min      2.9633
_cell_volume                     6704.6(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  'olex2.refine (Bourhis et al., 2015)'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.8686
_diffrn_measurement_details
;
  1 omega   39.00   94.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2277  178.0000 -150.0000 55

  2 omega  -75.00  -39.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3215 -178.0000  -60.0000 36

  3 omega  -68.00   -2.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3215  -57.0000 -150.0000 66

  4 omega  -40.00   49.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3215   77.0000  -30.0000 89
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0175081000
_diffrn_orient_matrix_UB_12      -0.0332962000
_diffrn_orient_matrix_UB_13      -0.0088300000
_diffrn_orient_matrix_UB_21      -0.0076191000
_diffrn_orient_matrix_UB_22      0.0147306000
_diffrn_orient_matrix_UB_23      -0.0377937000
_diffrn_orient_matrix_UB_31      0.0205117000
_diffrn_orient_matrix_UB_32      0.0339014000
_diffrn_orient_matrix_UB_33      0.0077480000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17704
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         30.14
_diffrn_reflns_theta_min         2.97
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.311
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93862
_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_density_diffrn    1.6763
_exptl_crystal_F_000             3337.4000
_refine_diff_density_max         1.6235
_refine_diff_density_min         -1.0567
_refine_diff_density_rms         0.1722
_refine_ls_d_res_high            0.7076
_refine_ls_d_res_low             6.8602
_refine_ls_goodness_of_fit_ref   1.0854
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    47
_refine_ls_number_parameters     439
_refine_ls_number_reflns         8606
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.0821
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.0266
_refine_ls_shift/su_mean         0.0011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0805P)^2^+21.3588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1721
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              33
_reflns_limit_h_min              -36
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                6033
_reflns_number_total             8606
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6qi00508j2.cif
_cod_data_source_block           1
_cod_database_code               4349634
_reflns_odcompleteness_completeness 99.81
_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. Restrained distances
 C27-C28
 1.35 with sigma of 0.01
 C28-C29
 1.35 with sigma of 0.01
 C29-C30
 1.35 with sigma of 0.01
 C30-C31
 1.35 with sigma of 0.01
 C31-C32
 1.35 with sigma of 0.01
 C32-C33
 1.35 with sigma of 0.01
 C33-C34
 1.35 with sigma of 0.01
 C34-C35
 1.35 with sigma of 0.01
 C35-C36
 1.35 with sigma of 0.01
 C27-C36
 1.35 with sigma of 0.01
3. Rigid bond restraints
 C30, C31, C32, C33, C34, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
5.a :
 C29(C30,C31,C32,C33,C34)
5.b Me refined with riding coordinates:
 C1(H1a,H1b,H1c), C8(H8a,H8b,H8c)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C11(H11), C14(H14), C16(H16), C17(H17), C18(H18),
 C19(H19), C21(H21), C22(H22), C25(H25), C28(H28), C30(H30), C31(H31), C32(H32),
  C33(H33), C35(H35), C36(H36)
;
_olex2_submission_special_instructions 'No special instructions were received'