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_4349629
_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 Dy2 F12 O16, 2(H2 O)'
_chemical_formula_sum            'C74 H62 Dy2 F12 O18'
_chemical_formula_weight         1792.24
_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     iterative
_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                105.513(5)
_cell_angle_beta                 101.950(4)
_cell_angle_gamma                111.582(5)
_cell_formula_units_Z            1
_cell_length_a                   10.4693(5)
_cell_length_b                   14.2053(8)
_cell_length_c                   14.5234(7)
_cell_measurement_reflns_used    6553
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0951
_cell_measurement_theta_min      3.0198
_cell_volume                     1819.4(2)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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 0.997
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_details
;
  1 omega   -5.00   88.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0103   77.0000    0.0000 93

  2 omega   42.00   68.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0103   19.0000   90.0000 26

  3 omega  -51.00   35.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0103  -57.0000 -120.0000 86

  4 omega    5.00   59.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0103   57.0000 -120.0000 54

  5 omega  -47.00   48.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1040   77.0000  120.0000 95

  6 omega  -25.00   21.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1040  -99.0000    0.0000 46
;
_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      0.0132569000
_diffrn_orient_matrix_UB_12      0.0072574000
_diffrn_orient_matrix_UB_13      0.0519228000
_diffrn_orient_matrix_UB_21      -0.0215891000
_diffrn_orient_matrix_UB_22      -0.0567462000
_diffrn_orient_matrix_UB_23      -0.0131356000
_diffrn_orient_matrix_UB_31      0.0732423000
_diffrn_orient_matrix_UB_32      0.0095095000
_diffrn_orient_matrix_UB_33      0.0061760000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15001
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         3.03
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    2.138
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87950
_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    1.636
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             890
_refine_diff_density_max         1.631
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         8216
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+3.1105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                7003
_reflns_number_total             8216
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00508j4.cif
_cod_data_source_block           1
_cod_original_cell_volume        1819.40(16)
_cod_database_code               4349629
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All O(H,H) groups
2. Restrained distances
 O8-H8
 0.85 with sigma of 0.01
 C26-C27
 1.35 with sigma of 0.01
 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
 C26-C35
 1.35 with sigma of 0.01
 Dy1-H8
 2.865918 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
4.a Riding coordinates:
 O8(H8), O9(H9A,H9B)
4.b Me refined with riding coordinates:
 C37(H37A,H37B,H37C)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C10(H10), C13(H13), C16(H16), C17(H17), C18(H18),
 C19(H19), C21(H21), C24(H24), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
  C33(H33), C35(H35), C36(H36)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C)
;
_olex2_submission_special_instructions 'No special instructions were received'