Modulation of magnetic relaxation behaviors via replacing coordinated solvents in a series of linear tetranuclear Dy4 complexes
Wang, Wen-Min; Hu, Xin-Yan; Yang, Yang; Zhao, Jia-Qi; Zhang, Ya-Xin; Kang, Xiao-Min; Wu, Zhi-Lei; New Journal of Chemistry 44 (2020) 8494–8502; doi:10.1039/D0NJ01830A

data_7059569
_publ_section_title
;
 Modulation of magnetic relaxation behaviors via replacing coordinated
 solvents in a series of linear tetranuclear Dy4 complexes
;
_journal_issue                   20
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8494
_journal_page_last               8502
_journal_paper_doi               10.1039/D0NJ01830A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C120 H94 Dy4 N6 O22, 4(C H4 O)'
_chemical_formula_sum            'C124 H110 Dy4 N6 O26'
_chemical_formula_weight         2750.17
_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
_audit_creation_date             2020-04-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-03 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                96.328(3)
_cell_angle_beta                 111.526(3)
_cell_angle_gamma                114.217(3)
_cell_formula_units_Z            1
_cell_length_a                   14.2043(10)
_cell_length_b                   15.2626(12)
_cell_length_c                   16.5652(14)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.37
_cell_volume                     2899.3(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_av_unetI/netI     0.0828
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43601
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.368
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.623
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0931 before and 0.0643 after correction.
The Ratio of minimum to maximum transmission is 0.6912.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.940
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         11339
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0735P)^2^+2.6421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7614
_reflns_number_total             11339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01830a2.cif
_cod_data_source_block           1
_cod_depositor_comments
;Adding full bibliography for 7059569--7059572.cif.

 Adding full bibliography for 7059569--7059572.cif.
;
_cod_database_code               7059569
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.572
_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
 O11-H11
 0.87 with sigma of 0.01
 H13-H11
 2.2 with sigma of 0.02
 O9-H13
 2.5 with sigma of 0.02
 O4-H4
 0.87 with sigma of 0.01
 C60-H11
 1.887779 with sigma of 0.02
 Dy1-H11
 2.986666 with sigma of 0.02
 C14-H4
 1.891745 with sigma of 0.02
 Dy2-H4
 2.970423 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C15A) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C17A) \\sim Ueq,
Uanis(C17B) \\sim Ueq, Uanis(C16B) \\sim Ueq, Uanis(C15B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15A) = Uanis(C15B) = Uanis(C16B) = Uanis(C16A) = Uanis(C17A) =
Uanis(C17B)
4. Others
 Sof(H18A)=Sof(C15B)=Sof(H15B)=Sof(C16B)=Sof(H16B)=Sof(C17B)=Sof(H17B)=1-FVAR(1)
 Sof(H18)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C7(H7), C30(H30), C49(H49), C3(H3), C4(H4A), C12(H12), C11(H11A),
 C5(H5), C57(H57), C55(H55), C34(H34), C56(H56), C59(H59), C19(H19), C22(H22),
 C33(H33), C48(H48), C44(H44), C37(H37), C26(H26), C27(H27), C18(H18),
 C18(H18A), C43(H43), C29(H29), C25(H25), C58(H58), C41(H41), C31(H31),
 C52(H52), C47(H47), C40(H40), C28(H28), C42(H42), C32(H32), C45(H45), C46(H46),
  C15A(H15A), C16A(H16A), C17A(H17A), C15B(H15B), C16B(H16B), C17B(H17B)
5.c Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C61(H61A,H61B,H61C)
5.d Idealised tetrahedral OH refined as rotating group:
 O12(H12A), O13(H13)
;
_shelx_res_checksum              74530
_shelx_fab_checksum              88092
_olex2_submission_special_instructions 'No special instructions were received'