Counter anions influence the relaxation dynamics of phenoxy-bridged Dy<sub>2</sub> single molecule magnets.
Liu, Shuting; Lu, Jingjing; Li, Xiao-Lei; Zhu, Zhenhua; Tang, Jinkui; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12372–12379; doi:10.1039/d0dt02451a

data_7705027
_publ_section_title
;
 Counter anions influence the relaxation dynamics of phenoxy-bridged
 Dy<sub>2</sub> single molecule magnets.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12372
_journal_page_last               12379
_journal_paper_doi               10.1039/d0dt02451a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C53 H50 Dy2 N12 O10, 2(Cl O4), 4(C H4 O), 2(H2 O)'
_chemical_formula_sum            'C57 H70 Cl2 Dy2 N12 O24'
_chemical_formula_weight         1703.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6143)
;
_audit_update_record
;
2020-08-03 deposited with the CCDC.	2020-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.9210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0961(9)
_cell_length_b                   18.9669(12)
_cell_length_c                   26.3438(18)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      26.10
_cell_measurement_theta_min      2.29
_cell_volume                     6805.8(8)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.638
_diffrn_measured_fraction_theta_max 0.658
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_Laue_measured_fraction_full 0.638
_diffrn_reflns_Laue_measured_fraction_max 0.658
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26112
_diffrn_reflns_point_group_measured_fraction_full 0.638
_diffrn_reflns_point_group_measured_fraction_max 0.658
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.109
_diffrn_reflns_theta_min         1.339
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.343
_exptl_absorpt_correction_T_max  0.288
_exptl_absorpt_correction_T_min  0.136
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       block
_exptl_crystal_F_000             3416
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.378
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         8915
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0694P)^2^+28.7539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1517
_refine_ls_wR_factor_ref         0.1595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7238
_reflns_number_total             8915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02451a2.cif
_cod_data_source_block           Dy2-ClO4
_cod_depositor_comments
'Adding full bibliography for 7705026--7705029.cif.'
_cod_database_code               7705027
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.799
_shelx_estimated_absorpt_t_min   0.651
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(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
 O13-C57
 1.43 with sigma of 0.01
 O11-C56
 1.43 with sigma of 0.01
 C55-O16
 1.43 with sigma of 0.01
 O15-C54
 1.43 with sigma of 0.01
 O5-H5
 0.85 with sigma of 0.01
 H12D-O12
 0.82 with sigma of 0.01
 Cl2-O1A = Cl2-O1B = Cl2-O1C = Cl2-O1D
 1.5 with sigma of 0.02
 Dy1-H5
 2.864755 with sigma of 0.02
 C35-H5
 1.870334 with sigma of 0.02
 O1A-O1C \\sim O1B-O1D \\sim O1A-O1D \\sim O1B-O1C \\sim O1A-O1B \\sim O1C-O1D
 with sigma of 0.04
 Cl2-O1A \\sim Cl2-O1B \\sim Cl2-O1C \\sim Cl2-O1D
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim O1A \\sim O1B \\sim O1C \\sim O1D: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(O14) \\sim Ueq, Uanis(C55) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 Cl2, O1A, O1B, O1C, O1D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Everything fixed:
 O14, H14A, H14B
5.b Riding coordinates:
 O11(H11A), O13(H13), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C57(H12D,H12E)
5.c Rotating group:
 O6(H6A,H6B)
5.d Aromatic/amide H refined with riding coordinates:
 N2(H2), C1(H1), C2(H2A), N11(H11), N5(H5A), C4(H4), C5(H5B), C7(H7), C8(H8),
 C9(H9), C10(H10), N8(H8A), C15(H15), C18(H18), C21(H21), C22(H22), C24(H24),
 C26(H26), C28(H28), C31(H31), C33(H33), C34(H34), C37(H37), C38(H38), C41(H41),
  C42(H42), C43(H43), C44(H44), C49(H49), C51(H51), C52(H52), C53(H53)
5.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C17(H17A,H17B,H17C), C35(H35A,H35B,H35C), C40(H40A,H40B,
 H40C), C46(H46A,H46B,H46C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C)
5.f Idealised tetrahedral OH refined as rotating group:
 O15(H15A), O16(H16)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82139
_shelx_fab_checksum              95896
_olex2_submission_special_instructions 'No special instructions were received'