Modulating single-molecule magnet behavior towards multiple magnetic relaxation processes through structural variation in Dy4 clusters
Wang, Wen-Min; Kang, Xiao-Min; Shen, Hai-Yun; Wu, Zhi-Lei; Gao, Hong-Ling; Cui, Jian-Zhong; Inorganic Chemistry Frontiers 5 (2018) 1876–; doi:10.1039/C8QI00214B

data_4349843
_publ_section_title
;
 Modulating single-molecule magnet behavior towards multiple magnetic
 relaxation processes through structural variation in Dy4 clusters
;
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1876
_journal_paper_doi               10.1039/C8QI00214B
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         'C116 H180 Dy4 N8 O24, 2(C O)'
_chemical_formula_sum            'C118 H180 Dy4 N8 O26'
_chemical_formula_weight         2776.69
_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             2018-02-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-21 deposited with the CCDC.
2018-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                77.6670(10)
_cell_angle_beta                 77.7820(10)
_cell_angle_gamma                68.5510(10)
_cell_formula_units_Z            1
_cell_length_a                   12.2174(4)
_cell_length_b                   15.9283(6)
_cell_length_c                   19.3779(7)
_cell_measurement_reflns_used    16524
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      3.1
_cell_volume                     3391.7(2)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            75493
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         3.028
_exptl_absorpt_coefficient_mu    2.243
_exptl_absorpt_correction_T_max  0.8723
_exptl_absorpt_correction_T_min  0.6722
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.116
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         11939
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0468P)^2^+21.3952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1393
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9398
_reflns_number_total             11939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00214b2.cif
_cod_data_source_block           111
_cod_database_code               4349843
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.775
_shelx_estimated_absorpt_t_min   0.534
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O12-H12
 0.85 with sigma of 0.01
 C58-H12
 1.853504 with sigma of 0.02
3. Rigid bond restraints
 C58, O12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C55, C54
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C28, C27, C26, C25
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C26, C28, C25, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C32, C33, C35, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(C58) \\sim Ueq, Uanis(O12) \\sim Ueq: 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(C15)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C25) \\sim Ueq,
Uanis(C27) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C36) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O0AA) \\sim Ueq, Uanis(C0AA) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C54) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C52(H52), C8(H8), C10(H10), C9(H9), C4(H4), C3(H3A), C2(H2), C19(H19),
 C41(H41), C30(H30)
5.b Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C16(H16A,H16B,H16C), C34(H34A,H34B,H34C), C37(H37A,H37B,
 H37C), C49(H49A,H49B,H49C), C24(H24A,H24B,H24C), C35(H35A,H35B,H35C), C48(H48A,
 H48B,H48C), C44(H44A,H44B,H44C), C22(H22A,H22B,H22C), C36(H36A,H36B,H36C),
 C23(H23A,H23B,H23C), C14(H14A,H14B,H14C), C26(H26A,H26B,H26C), C38(H38A,H38B,
 H38C), C27(H27A,H27B,H27C), C25(H25A,H25B,H25C), C55(H55A,H55B,H55C), C13(H13A,
 H13B,H13C), C33(H33A,H33B,H33C), C57(H57A,H57B,H57C), C45(H45A,H45B,H45C),
 C56(H56A,H56B,H56C), C15(H15A,H15B,H15C), C47(H47A,H47B,H47C), C58(H58A,H58B,
 H58C)
5.c Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              10822
_shelx_hkl_checksum              29491
_olex2_submission_special_instructions 'No special instructions were received'