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_4349631
_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         'C74 H58 F12 Gd2 O16, 2(O)'
_chemical_formula_sum            'C74 H58 F12 Gd2 O18'
_chemical_formula_weight         1777.70
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-02-29
_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                65.464(7)
_cell_angle_beta                 78.393(7)
_cell_angle_gamma                68.374(7)
_cell_formula_units_Z            1
_cell_length_a                   10.5094(9)
_cell_length_b                   14.2002(10)
_cell_length_c                   14.5239(11)
_cell_measurement_reflns_used    6959
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6332
_cell_measurement_theta_min      3.0944
_cell_volume                     1830.0(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 0.882
_diffrn_measurement_details
;
  1 omega  -25.00   22.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6768  -99.0000    0.0000 47

  2 omega  -96.00  -20.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6768  -57.0000   60.0000 76

  3 omega  -89.00  -59.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6768 -178.0000 -120.0000 30

  4 omega  -61.00   19.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6768   77.0000 -180.0000 80

  5 omega  -34.00    1.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6768  -84.0000 -111.0000 35

  6 omega  -30.00   24.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6768   38.0000  -90.0000 54

  7 omega  -99.00   40.00   1.0000   17.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.6768    0.0000 -120.0000 139
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0454986000
_diffrn_orient_matrix_UB_12      0.0293672000
_diffrn_orient_matrix_UB_13      0.0293630000
_diffrn_orient_matrix_UB_21      -0.0082355000
_diffrn_orient_matrix_UB_22      -0.0494018000
_diffrn_orient_matrix_UB_23      0.0372671000
_diffrn_orient_matrix_UB_31      0.0561247000
_diffrn_orient_matrix_UB_32      -0.0074534000
_diffrn_orient_matrix_UB_33      0.0253072000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15821
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.70
_diffrn_reflns_theta_min         3.10
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    1.896
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91533
_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            'dull light orange'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             882
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.429
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         9161
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+2.1438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1237
_reflns_number_gt                7727
_reflns_number_total             9161
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00508j4.cif
_cod_data_source_block           thr-146
_cod_original_cell_volume        1830.0(2)
_cod_database_code               4349631
_reflns_odcompleteness_completeness 99.82
_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, All O(H) groups
2. Restrained distances
 O8-H8
 0.85 with sigma of 0.01
 C11-C10 = C10-C9
 1.4 with sigma of 0.02
 C1A-C2A = C3A-C6A = C4AB-C3AB
 1.4 with sigma of 0.02
 C37-H8
 1.851983 with sigma of 0.02
 Gd1-H8
 2.885286 with sigma of 0.02
3. Others
 Sof(C4A)=Sof(H4A)=Sof(C0AB)=Sof(C1AB)=Sof(H1AB)=Sof(C4AB)=Sof(H4AB)=Sof(C3AB)=
 Sof(C6A)=Sof(H6A)=Sof(C3A)=Sof(H3A)=Sof(C2A)=Sof(H2A)=Sof(C1A)=Sof(H1A)=
 Sof(C2AB)=1-FVAR(1)
 Sof(C5)=Sof(C14)=Sof(H14)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(C12)=Sof(C13)=Sof(H13)=
 Sof(C8)=Sof(H8A)=Sof(C11)=Sof(H11)=Sof(C10)=Sof(H10)=Sof(C9)=Sof(H9)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C30(H30), C32(H32), C27(H27), C3(H3), C31(H31), C19(H19), C20(H20),
 C23(H23), C22(H22), C24(H24), C25(H25), C14(H14), C6(H6), C13(H13), C8(H8A),
 C11(H11), C10(H10), C9(H9), C4A(H4A), C1AB(H1AB), C4AB(H4AB), C6A(H6A),
 C3A(H3A), C2A(H2A), C1A(H1A)
4.b Idealised Me refined as rotating group:
 C28(H28a,H28b,H28c), C35(H35a,H35b,H35c), C37(H37a,H37b,H37c)
;
_olex2_submission_special_instructions 'No special instructions were received'