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_7705949
_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         'C80 H92 Dy4 N32 O8, 16(Cl0.5 O2), 11(O)'
_chemical_formula_sum            'C80 H114 Cl8 Dy4 N32 O51'
_chemical_formula_weight         3273.63
_space_group_crystal_system      cubic
_space_group_IT_number           223
_space_group_name_Hall           '-P 4n 2 3'
_space_group_name_H-M_alt        'P m -3 n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc25fv6p
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   26.8985(3)
_cell_length_b                   26.8985(3)
_cell_length_c                   26.8985(3)
_cell_measurement_reflns_used    9762
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      62.28
_cell_measurement_theta_min      2.32
_cell_volume                     19461.9(4)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.882
_diffrn_measured_fraction_theta_max 0.999
_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  0.0728
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.882
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            57622
_diffrn_reflns_point_group_measured_fraction_full 0.882
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         62.333
_diffrn_reflns_theta_min         2.323
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    14.460
_exptl_absorpt_correction_T_max  0.141
_exptl_absorpt_correction_T_min  0.074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. Rint was 0.1482 before and 0.0728 after correction. The Ratio of minimum to maximum transmission is 0.5248. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_description       block
_exptl_crystal_F_000             9756
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.002
_refine_diff_density_min         -2.238
_refine_diff_density_rms         0.257
_refine_ls_extinction_coef       0.00012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.213
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2781
_refine_ls_number_restraints     361
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.1058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1148P)^2^+801.4122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2874
_refine_ls_wR_factor_ref         0.2915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2520
_reflns_number_total             2781
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02869j2.cif
_cod_data_source_block           Dy4
_cod_depositor_comments
'Adding full bibliography for 7705949--7705952.cif.'
_cod_original_cell_volume        19461.8(7)
_cod_database_code               7705949
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.181
_shelx_estimated_absorpt_t_min   0.181
_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
2. Restrained distances
 Cl1-O5 = Cl1-O7 = Cl1-O8 = Cl1-O10 = Cl2-O9
 1.5 with sigma of 0.02
 Dy1-H1
 2.882846 with sigma of 0.02
 O6-O9
 2.3 with sigma of 0.04
 Cl1-O5 \\sim Cl1-O7 \\sim Cl1-O8 \\sim Cl1-O10
 with sigma of 0.02
 O5-O8 \\sim O7-O10 \\sim O5-O10 \\sim O7-O8 \\sim O5-O7 \\sim O8-O10
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O7 \\sim O8 \\sim O5 \\sim O10 \\sim O9 \\sim O6 \\sim O3 \\sim O2: within 38A
with sigma of 0.1 and sigma for terminal atoms of 0.2 within 38A
Cl1 \\sim Cl2 \\sim Cl00: within 38A with sigma of 0.05 and sigma for terminal
atoms of 0.1 within 38A
Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N1) \\sim
Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O6)
\\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O7) \\sim Ueq,
Uanis(O8) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O11)
\\sim Ueq, Uanis(Cl00) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl1) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 O6, Cl2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl1, O5, O7, O8, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, O9, Cl2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(O13A)=0.25*(1-FVAR(2))
 Sof(O12A)=0.125*(1-FVAR(2))
 Sof(O12)=0.125*FVAR(2)
 Sof(O13)=0.25*FVAR(2)
 Fixed Sof: H11A(0.5) H11B(0.5) H11C(0.5) Cl1(0.5) O5(0.5) O7(0.5) O8(0.5)
 O10(0.5)
6.a Riding coordinates:
 C7(H7A,H7B,H7C), C11(H11A,H11B,H11C)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
6.c Aromatic/amide H refined with riding coordinates:
 O1(H1), C4(H4), C3(H3), C5(H5), C8(H8)
6.d Fitted hexagon refined as free rotating group:
 C4(C3,C2,N1,C6,C5)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'