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_7705029
_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
'C54 H52 Dy2 N12 O10, 2(C F3 O3 S), 0.5(C H2 Cl2), 3(C H4 O), 0.5(C H3 O)'
_chemical_formula_sum            'C60 H62.5 Cl Dy2 F6 N12 O19.5 S2'
_chemical_formula_weight         1806.32
_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   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                95.9670(10)
_cell_angle_beta                 100.081(2)
_cell_angle_gamma                90.9640(10)
_cell_formula_units_Z            4
_cell_length_a                   15.7602(13)
_cell_length_b                   18.2693(15)
_cell_length_c                   24.804(2)
_cell_measurement_reflns_used    9600
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      58.95
_cell_measurement_theta_min      3.98
_cell_volume                     6988.9(10)
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_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  0.0270
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            43444
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.045
_diffrn_reflns_theta_min         0.839
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.315
_exptl_absorpt_correction_T_max  0.357
_exptl_absorpt_correction_T_min  0.246
_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    1.717
_exptl_crystal_description       block
_exptl_crystal_F_000             3606
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.153
_refine_diff_density_min         -1.625
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1883
_refine_ls_number_reflns         27313
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+17.9911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1168
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23369
_reflns_number_total             27313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02451a2.cif
_cod_data_source_block           Dy2-CF3SO3
_cod_depositor_comments
;
Adding full bibliography for 7705026--7705029.cif.

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C120 H133 Cl2 Dy4 F12 N24 O39 S4'
_cod_original_formula_weight         3612.64
_cod_original_formula_moiety
'2(C54 H52 Dy2 N12 O10), 4(C F3 O3 S), C H2 Cl2, 6(C H4 O), C H3 O'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        6989.1(10)
_cod_database_code               7705029
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.802
_shelx_estimated_absorpt_t_min   0.723
_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
2. Restrained distances
 C114-O37
 1.43 with sigma of 0.01
 O6-H6
 0.85 with sigma of 0.01
 O34-C116
 1.43 with sigma of 0.01
 C115-O33
 1.43 with sigma of 0.01
 C119-O35
 1.43 with sigma of 0.01
 C118-O38
 1.43 with sigma of 0.01
 O36-C117
 1.43 with sigma of 0.01
 O17-H17
 0.85 with sigma of 0.01
 O5-H5
 0.85 with sigma of 0.01
 O21-H21
 0.85 with sigma of 0.01
 O39-C120
 1.43 with sigma of 0.01
 Dy2-O4
 2.4 with sigma of 0.01
 C111-H6
 2.049627 with sigma of 0.02
 Dy2-H6
 3.03162 with sigma of 0.02
 Dy1-H5
 2.859937 with sigma of 0.02
 C105-H17
 1.899453 with sigma of 0.02
 Dy4-H17
 2.884764 with sigma of 0.02
 C109-H21
 1.902484 with sigma of 0.02
 Dy3-H21
 2.875728 with sigma of 0.02
 C107-H5
 1.893067 with sigma of 0.02
3. Rigid bond restraints
 C111, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C113, F12, F10, F11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C111 \\sim O6: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C113 \\sim F12 \\sim F11 \\sim F10: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(C111) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5.a Secondary CH2 refined with riding coordinates:
 C112(H11V,H11W)
5.b Aromatic/amide H refined with riding coordinates:
 N17(H17A), N5(H5A), N8(H8), N23(H23A), N2(H2), N14(H14), N20(H20), N11(H11),
 C2(H2A), C3(H3), C6(H6A), C15(H15), C16(H16), C19(H19), C20(H20A), C21(H21A),
 C23(H23), C25(H25), C26(H26), C31(H31), C33(H33), C35(H35), C36(H36), C39(H39),
  C40(H40), C41(H41), C42(H42), C45(H45), C50(H50), C51(H51), C55(H55),
 C57(H57), C59(H59), C60(H60), C62(H62), C64(H64), C68(H68), C70(H70), C71(H71),
  C73(H73), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80),
 C81(H81), C82(H82), C84(H84), C85(H85), C87(H87), C90(H90), C91(H91), C92(H92),
  C93(H93), C94(H94), C95(H95), C96(H96), C97(H97), C98(H98), C99(H99),
 C101(H101), C102(H102), C104(H104)
5.c Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C66(H66A,H66B,H66C), C83(H83A,H83B,H83C), C86(H86A,H86B,
 H86C), C88(H88A,H88B,H88C), C100(H10J,H10K,H10L), C103(H10A,H10B,H10C),
 C105(H10M,H10N,H10O), C106(H10D,H10E,H10F), C107(H10G,H10H,H10I), C109(H10P,
 H10Q,H10R), C111(H11A,H11B,H11C), C114(H11P,H11Q,H11R), C115(H11D,H11E,H11F),
 C116(H11G,H11H,H11I), C117(H11M,H11N,H11O), C118(H11S,H11T,H11U), C119(H11J,
 H11K,H11L), C120(H12A,H12B,H12C)
5.d Idealised tetrahedral OH refined as rotating group:
 O33(H33A), O34(H34), O35(H35A), O36(H36A), O37(H37), O38(H38)
;
_shelx_res_checksum              25462
_shelx_fab_checksum              60105
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'