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_7705950
_publ_section_title
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 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
'C21 H27 Dy2 N13 O18, 1.77(C2 H3 N), 1.23(C H4 O)'
_chemical_formula_sum            'C25.77 H37.23 Dy2 N14.77 O19.23'
_chemical_formula_weight         1186.63
_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     dual
_audit_block_doi                 10.5517/ccdc.csd.cc25fv5n
_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                63.1760(10)
_cell_angle_beta                 88.7940(10)
_cell_angle_gamma                79.8230(10)
_cell_formula_units_Z            2
_cell_length_a                   11.6126(3)
_cell_length_b                   13.7845(4)
_cell_length_c                   14.7071(4)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    173
_cell_measurement_theta_max      66.68
_cell_measurement_theta_min      3.38
_cell_volume                     2063.23(10)
_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      173.0
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.993
_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  0.0614
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23881
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.678
_diffrn_reflns_theta_min         3.375
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    19.983
_exptl_absorpt_correction_T_max  0.069
_exptl_absorpt_correction_T_min  0.050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. Rint was 0.0779 before and 0.0614 after correction. The Ratio of minimum to maximum transmission is 0.7246. 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    1.910
_exptl_crystal_description       block
_exptl_crystal_F_000             1162
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.858
_refine_diff_density_min         -1.643
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         7259
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0358P)^2^+9.5908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6342
_reflns_number_total             7259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02869j2.cif
_cod_data_source_block           Dy2
_cod_depositor_comments
'Adding full bibliography for 7705949--7705952.cif.'
_cod_database_code               7705950
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.154
_shelx_estimated_absorpt_t_min   0.123
_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
 O23A-C27
 1.45 with sigma of 0.02
 Dy1-H2
 2.984202 with sigma of 0.02
 Dy2-H1
 3.022075 with sigma of 0.02
 Dy1-H3
 2.898667 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O23A) \\sim Ueq, Uanis(N15) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C27, O23A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(O23A)=Sof(H23D)=1-FVAR(1)
 Sof(N14)=Sof(C23B)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C20(H20A,H20B)
6.b Aromatic/amide H refined with riding coordinates:
 O1(H1), O2(H2), O3(H3), C3(H3A), C4(H4), C5(H5), C8(H8), C13(H13), C16(H16),
 C17(H17), C18(H18)
6.c Tetrahedral OH refined with riding coordinates:
 O19(H19)
6.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C21(H21A,H21B,
 H21C), C23B(H23A,H23B,H23C), C25(H25A,H25B,H25C), C22(H22A,H22B,H22C),
 C27(H27A,H27B,H27C)
6.e Idealised tetrahedral OH refined as rotating group:
 O23A(H23D)
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_olex2_submission_special_instructions 'No special instructions were received'