Single-molecule magnets under dc field with an anion effect: self-assembly of pure dysprosium(iii) metallacycles.
Wu, Jianfeng; Yang, Qianqian; Wang, Haoyu; Ge, Yan; Tang, Jinkui; Qi, Zhenhui; Dalton transactions (Cambridge, England : 2003) 50 (2021) 262–269; doi:10.1039/d0dt02869j

data_7705952
_publ_section_title
;
 Single-molecule magnets under dc field with an anion effect:
 self-assembly of pure dysprosium(iii) metallacycles.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              262
_journal_page_last               269
_journal_paper_doi               10.1039/d0dt02869j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C81 H91 Dy4 F3 N32 O11 S, 6(C F3 O3 S), 2(H2 O), 2(C2 H3 N), C0.5 F3 O3 S'
_chemical_formula_sum            'C91.5 H101 Dy4 F24 N34 O34 S8'
_chemical_formula_weight         3583.54
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc25fv7q
_audit_creation_date             2020-11-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-11-09 deposited with the CCDC.	2020-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.012(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.3943(8)
_cell_length_b                   26.5959(9)
_cell_length_c                   43.3898(14)
_cell_measurement_reflns_used    9225
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      58.77
_cell_measurement_theta_min      2.69
_cell_volume                     29143.6(16)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.779
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.779
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            91490
_diffrn_reflns_point_group_measured_fraction_full 0.779
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         58.928
_diffrn_reflns_theta_min         2.048
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    12.820
_exptl_absorpt_correction_T_max  0.188
_exptl_absorpt_correction_T_min  0.112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. Rint was 0.1079 before and 0.0527 after correction. The Ratio of minimum to maximum transmission is 0.5957. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       block
_exptl_crystal_F_000             14144
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.489
_refine_diff_density_min         -1.751
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1912
_refine_ls_number_reflns         20521
_refine_ls_number_restraints     527
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0667
_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^)+(0.1115P)^2^+488.4250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1837
_refine_ls_wR_factor_ref         0.1919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17527
_reflns_number_total             20521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02869j2.cif
_cod_data_source_block           Dy4_CF3SO3
_cod_depositor_comments
'Adding full bibliography for 7705949--7705952.cif.'
_cod_original_formula_sum        'C91.50 H101 Dy4 F24 N34 O34 S8'
_cod_database_code               7705952
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.219
_shelx_estimated_absorpt_t_min   0.206
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,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
 C87-S3
 1.75 with sigma of 0.02
 C90-S4
 1.75 with sigma of 0.02
 S7-C88
 1.75 with sigma of 0.02
 S1-C85
 1.75 with sigma of 0.02
 C92-S2
 1.75 with sigma of 0.02
 C87-F14
 1.35 with sigma of 0.02
 C87-F13
 1.35 with sigma of 0.02
 C87-F15
 1.35 with sigma of 0.02
 C90-F10
 1.35 with sigma of 0.02
 C90-F11
 1.35 with sigma of 0.02
 C90-F12
 1.35 with sigma of 0.02
 C89-F24
 1.35 with sigma of 0.02
 C89-F22
 1.35 with sigma of 0.02
 C89-F23
 1.35 with sigma of 0.02
 S8-O28
 1.44 with sigma of 0.02
 S8-O27
 1.44 with sigma of 0.02
 S8-O29
 1.44 with sigma of 0.02
 S8-C89
 1.75 with sigma of 0.02
 S0AA-O2BA
 1.45 with sigma of 0.02
 S0AA-O2AA
 1.45 with sigma of 0.02
 S0AA-O3AA
 1.45 with sigma of 0.02
 C1AA-F58
 1.35 with sigma of 0.02
 C1AA-F40
 1.35 with sigma of 0.02
 C1AA-F41
 1.35 with sigma of 0.02
 C89A-F22A
 1.35 with sigma of 0.02
 C89A-F24A
 1.35 with sigma of 0.02
 C89A-F23A
 1.35 with sigma of 0.02
 O1-H1
 0.87 with sigma of 0.01
 O2-H2
 0.87 with sigma of 0.01
 O3-H3
 0.87 with sigma of 0.01
 O4-H4
 0.87 with sigma of 0.01
 O5-H5
 0.87 with sigma of 0.01
 O6-H6
 0.87 with sigma of 0.01
 O7-H7
 0.87 with sigma of 0.01
 O8-H8
 0.87 with sigma of 0.01
 S6-O1A = S6-O1B = S6-O1C
 1.44 with sigma of 0.02
 C1A-F7 = C1A-F8 = C1A-F9
 1.33 with sigma of 0.02
 C1A-S6
 1.82 with sigma of 0.02
 H6-H36B
 2.2 with sigma of 0.02
 H7-H33A
 2.2 with sigma of 0.02
 F14-F15
 2.1 with sigma of 0.04
 F14-F13
 2.1 with sigma of 0.04
 F15-F13
 2.1 with sigma of 0.04
 F10-F11
 2.1 with sigma of 0.04
 F10-F12
 2.1 with sigma of 0.04
 F12-F11
 2.1 with sigma of 0.04
 F24-F22
 2.1 with sigma of 0.04
 F24-F23
 2.1 with sigma of 0.04
 F23-F22
 2.1 with sigma of 0.04
 F24-S8
 2.6 with sigma of 0.02
 S8-F22
 2.6 with sigma of 0.04
 S8-F23
 2.6 with sigma of 0.04
 C89-O28
 2.5 with sigma of 0.04
 C89-O27
 2.5 with sigma of 0.04
 C89-O29
 2.5 with sigma of 0.04
 C1AA-O2BA
 2.5 with sigma of 0.04
 C1AA-O3AA
 2.5 with sigma of 0.04
 C1AA-O2AA
 2.5 with sigma of 0.04
 S0AA-F58
 2.56 with sigma of 0.04
 S0AA-F41
 2.56 with sigma of 0.04
 S0AA-F40
 2.56 with sigma of 0.04
 F24A-F22A
 2.1 with sigma of 0.04
 F22A-F23A
 2.1 with sigma of 0.04
 F23A-F24A
 2.1 with sigma of 0.04
 S8A-F23A
 2.6 with sigma of 0.04
 S8A-F22A
 2.6 with sigma of 0.04
 S8A-F24A
 2.6 with sigma of 0.04
 C1-H1
 1.898188 with sigma of 0.02
 Dy1-H1
 2.927169 with sigma of 0.02
 C20-H2
 1.90837 with sigma of 0.02
 Dy4-H2
 3.028441 with sigma of 0.02
 C21-H3
 1.911069 with sigma of 0.02
 Dy4-H3
 3.016849 with sigma of 0.02
 C40-H4
 1.879031 with sigma of 0.02
 Dy3-H4
 2.929441 with sigma of 0.02
 C41-H5
 1.919957 with sigma of 0.02
 Dy3-H5
 2.930575 with sigma of 0.02
 C61-H6
 1.920207 with sigma of 0.02
 Dy2-H6
 2.909913 with sigma of 0.02
 C60-H7
 1.912619 with sigma of 0.02
 Dy2-H7
 2.919392 with sigma of 0.02
 C80-H8
 1.895937 with sigma of 0.02
 Dy1-H8
 2.919699 with sigma of 0.02
 C1A-O1C
 2.57 with sigma of 0.04
 C1A-O1A
 2.58 with sigma of 0.04
 C1A-O1B
 2.56 with sigma of 0.04
 S0AA-O2AA \\sim S5-O24
 with sigma of 0.02
 S0AA-O2BA \\sim S5-O26
 with sigma of 0.02
 S0AA-O3AA \\sim S5-O25
 with sigma of 0.02
 S0AA-C1AA \\sim S5-C86
 with sigma of 0.02
 F40-C1AA \\sim F17-C86
 with sigma of 0.02
 F41-C1AA \\sim F16-C86
 with sigma of 0.02
 C1AA-F58 \\sim C86-F18
 with sigma of 0.02
 S0AA-F40 \\sim S5-F17
 with sigma of 0.04
 S0AA-F41 \\sim S5-F16
 with sigma of 0.04
 S0AA-F58 \\sim S5-F18
 with sigma of 0.04
 O2AA-O2BA \\sim O24-O26
 with sigma of 0.04
 O2AA-O3AA \\sim O24-O25
 with sigma of 0.04
 O2AA-C1AA \\sim O24-C86
 with sigma of 0.04
 O2BA-O3AA \\sim O26-O25
 with sigma of 0.04
 O2BA-C1AA \\sim O26-C86
 with sigma of 0.04
 O3AA-C1AA \\sim O25-C86
 with sigma of 0.04
 F40-F41 \\sim F17-F16
 with sigma of 0.04
 F40-F58 \\sim F17-F18
 with sigma of 0.04
 F41-F58 \\sim F16-F18
 with sigma of 0.04
 S8-O27 \\sim S8A-O27A
 with sigma of 0.02
 S8-O28 \\sim S8A-O28A
 with sigma of 0.02
 S8-O29 \\sim S8A-O29A
 with sigma of 0.02
 S8-C89 \\sim S8A-C89A
 with sigma of 0.02
 F22-C89 \\sim F22A-C89A
 with sigma of 0.02
 F23-C89 \\sim F23A-C89A
 with sigma of 0.02
 F24-C89 \\sim F24A-C89A
 with sigma of 0.02
 S8-F22 \\sim S8A-F22A
 with sigma of 0.04
 S8-F23 \\sim S8A-F23A
 with sigma of 0.04
 S8-F24 \\sim S8A-F24A
 with sigma of 0.04
 F22-F23 \\sim F22A-F23A
 with sigma of 0.04
 F22-F24 \\sim F22A-F24A
 with sigma of 0.04
 F23-F24 \\sim F23A-F24A
 with sigma of 0.04
 O27-O28 \\sim O27A-O28A
 with sigma of 0.04
 O27-O29 \\sim O27A-O29A
 with sigma of 0.04
 O27-C89 \\sim O27A-C89A
 with sigma of 0.04
 O28-O29 \\sim O28A-O29A
 with sigma of 0.04
 O28-C89 \\sim O28A-C89A
 with sigma of 0.04
 O29-C89 \\sim O29A-C89A
 with sigma of 0.04
 S6-F7 \\sim S6-F8 \\sim S6-F9
 with sigma of 0.04
 O1A-O1B \\sim O1B-O1C \\sim O1A-O1C
 with sigma of 0.04
 C1A-O1A \\sim C1A-O1B \\sim C1A-O1C
 with sigma of 0.04
 C1A-F7 \\sim C1A-F8 \\sim C1A-F9
 with sigma of 0.02
 F7-F8 \\sim F8-F9 \\sim F9-F7
 with sigma of 0.04
 S6-O1A \\sim S6-O1B \\sim S6-O1C
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1A \\sim F7 \\sim F8 \\sim F9 \\sim S6 \\sim O1A \\sim O1B \\sim O1C: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(F22) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(S8) \\sim Ueq, Uanis(O29)
\\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(F24) \\sim Ueq,
Uanis(F23) \\sim Ueq, Uanis(F58) \\sim Ueq, Uanis(S0AA) \\sim Ueq, Uanis(O2AA)
\\sim Ueq, Uanis(O2BA) \\sim Ueq, Uanis(O3AA) \\sim Ueq, Uanis(C1AA) \\sim Ueq,
Uanis(F40) \\sim Ueq, Uanis(F41) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(S3)
\\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(C87) \\sim Ueq,
Uanis(F15) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(N34)
\\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C83) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(F17) \\sim Ueq, Uanis(S8) \\sim Ueq, Uanis(O28) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C86) \\sim Ueq, Uanis(S8) \\sim Ueq, Uanis(O2AA) \\sim Ueq, Uanis(O24)
\\sim Ueq, Uanis(O33) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O2AA) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C80)
\\sim Ueq, Uanis(O27) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C90) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(N34) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O29A) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O28A)
\\sim Ueq, Uanis(F24A) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(O2AA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(S6) \\sim Ueq, Uanis(O1C) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(O1B)
\\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F8) \\sim Ueq,
Uanis(F7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F24) = Uanis(C89)
Uanis(C89) = Uanis(F23)
Uanis(O2AA) = Uanis(S0AA)
Uanis(F22A) = Uanis(C89A)
Uanis(C89A) = Uanis(S8A)
4. Rigid body (RIGU) restrains
 C1A, F7, F8, F9, S6, O1A, O1B, O1C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S6, O1C, O1A, O1B, C1A, F8, F7, F9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(S5)=Sof(F16)=Sof(F17)=Sof(F18)=Sof(O24)=Sof(O25)=Sof(O26)=Sof(C86)=1-
 FVAR(1)
 Sof(S0AA)=Sof(F40)=Sof(F41)=Sof(F58)=Sof(O2AA)=Sof(O3AA)=Sof(O2BA)=Sof(C1AA)=
 FVAR(1)
 Sof(C89A)=Sof(S8A)=Sof(O27A)=Sof(O28A)=Sof(O29A)=Sof(F22A)=Sof(F23A)=
 Sof(F24A)=1-FVAR(2)
 Sof(S8)=Sof(F22)=Sof(F23)=Sof(F24)=Sof(O27)=Sof(O28)=Sof(O29)=Sof(C89)=FVAR(2)
6.a Riding coordinates:
 O36(H36A,H36B), O33(H33A,H33B), S6(O1C,O1A,O1B)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C20(H20A,H20B), C21(H21A,H21B), C41(H41A,H41B), C60(H60A,H60B),
 C61(H61A,H61B), C80(H80A,H80B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4A), C5(H5A), C8(H8A), C13(H13), C16(H16), C17(H17), C18(H18),
 C23(H23), C24(H24), C25(H25), C28(H28), C33(H33), C36(H36), C37(H37), C38(H38),
  C40(H40), C43(H43), C44(H44), C45(H45), C48(H48), C53(H53), C56(H56),
 C57(H57), C58(H58), C63(H63), C64(H64), C65(H65), C68(H68), C73(H73), C76(H76),
  C77(H77), C78(H78)
6.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C27(H27A,H27B,
 H27C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C47(H47A,H47B,H47C), C52(H52A,
 H52B,H52C), C54(H54A,H54B,H54C), C67(H67A,H67B,H67C), C72(H72A,H72B,H72C),
 C74(H74A,H74B,H74C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'