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_7059572
_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         'C124 H102 Dy4 N6 O22, 2(C3 H8 O)'
_chemical_formula_sum            'C130 H118 Dy4 N6 O24'
_chemical_formula_weight         2798.30
_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     iterative
_audit_creation_date             2020-04-12
_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                97.430(3)
_cell_angle_beta                 112.097(3)
_cell_angle_gamma                112.311(3)
_cell_formula_units_Z            1
_cell_length_a                   14.7864(10)
_cell_length_b                   15.1898(10)
_cell_length_c                   16.7985(10)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.34
_cell_volume                     3066.8(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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_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  0.1049
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_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            60339
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         2.341
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.480
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0860 before and 0.0662 after correction.
The Ratio of minimum to maximum transmission is 0.8151.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       block
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.829
_refine_diff_density_min         -1.446
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         12000
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+54.1172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8384
_reflns_number_total             12000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01830a2.cif
_cod_data_source_block           3
_cod_depositor_comments
;Adding full bibliography for 7059569--7059572.cif.

 Adding full bibliography for 7059569--7059572.cif.
;
_cod_database_code               7059572
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.723
_shelx_estimated_absorpt_t_min   0.565
_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-H11A
 0.87 with sigma of 0.01
 C61-C62
 1.5 with sigma of 0.02
 H17A_$1-H62B_$2
 2.2 with sigma of 0.02
 H62C_$3-H17A_$4
 2.2 with sigma of 0.02
 H62A_$5-H58_$6
 2.15 with sigma of 0.02
 H17B_$7-H62B_$1
 2.13 with sigma of 0.02
 H60B-H62A
 2.2 with sigma of 0.02
 O4-H4
 0.87 with sigma of 0.01
 C60-H11A
 1.965886 with sigma of 0.02
 Dy1-H11A
 2.949717 with sigma of 0.02
 C14-H4
 1.887108 with sigma of 0.02
 Dy2-H4
 2.961912 with sigma of 0.02
3. Rigid bond restraints
 C62, C61, C60
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C58 \\sim C59 \\sim C54: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C62 \\sim C61 \\sim C60: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(C59) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C62) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C60) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C16B) = Uanis(C16A)
Uanis(C20A) = Uanis(C15A) = Uanis(C16A) = Uanis(C17A) = Uanis(C20B) =
Uanis(C15B) = Uanis(C17B)
5. Others
 Sof(H19A)=Sof(H18A)=Sof(C15A)=Sof(H15A)=Sof(C17A)=Sof(H17A)=Sof(C16A)=
 Sof(H16A)=Sof(C20A)=1-FVAR(1)
 Sof(H19)=Sof(H18)=Sof(C17B)=Sof(H17B)=Sof(C16B)=Sof(H16B)=Sof(C15B)=Sof(H15B)=
 Sof(C20B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C64(H64A,H64B), C63(H63A,H63B), C60(H60A,H60B), C61(H61A,H61B)
6.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C7(H7), C10(H10), C11(H11), C12(H12), C34(H34), C25(H25), C3(H3),
 C4(H4A), C5(H5), C52(H52), C33(H33), C22(H22), C45(H45), C28(H28), C59(H59),
 C58(H58), C57(H57), C56(H56), C55(H55), C30(H30), C48(H48), C40(H40), C27(H27),
  C49(H49), C44(H44), C41(H41), C29(H29), C26(H26), C42(H42), C46(H46),
 C47(H47), C31(H31), C32(H32), C43(H43), C19(H19), C19(H19A), C18(H18),
 C18(H18A), C17B(H17B), C16B(H16B), C15B(H15B), C15A(H15A), C17A(H17A),
 C16A(H16A)
6.c Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C54(C59,C58,C57,C56,C55), C19(C18,C17B,C16B,C15B,C20B)
6.d Idealised Me refined as rotating group:
 C65(H65A,H65B,H65C), C62(H62A,H62B,H62C)
6.e Idealised tetrahedral OH refined as rotating group:
 O12(H12A)
;
_shelx_res_checksum              31974
_olex2_submission_special_instructions 'No special instructions were received'