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_4349845
_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         'C72 H42 Dy4 F48 N10 O24, 0.5(C14)'
_chemical_formula_sum            'C79 H42 Dy4 F48 N10 O24'
_chemical_formula_weight         3077.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 103.707(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.7920(18)
_cell_length_b                   17.7736(16)
_cell_length_c                   17.3809(17)
_cell_measurement_reflns_used    17302
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      3.1
_cell_volume                     5339.8(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            53554
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         3.110
_exptl_absorpt_coefficient_mu    2.921
_exptl_absorpt_correction_T_max  0.8337
_exptl_absorpt_correction_T_min  0.7418
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2948
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.289
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     887
_refine_ls_number_reflns         12205
_refine_ls_number_restraints     366
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+8.3207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0655
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10873
_reflns_number_total             12205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00214b2.cif
_cod_data_source_block           m20151218h1
_cod_database_code               4349845
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.721
_shelx_estimated_absorpt_t_min   0.593
_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
 F5'-F6'
 2.1 with sigma of 0.01
 C33-F22 = C33-F23 = C33-F24 = C33-F22' = C33-F23' = C33-F24'
 1.36 with sigma of 0.01
 C18-F4 = C18-F5 = C18-F6 = C18-F4' = C18-F5'
 1.36 with sigma of 0.01
 C14-F1 = C14-F2 = C14-F3 = C14-F1' = C14-F2' = C14-F3'
 1.36 with sigma of 0.01
 C29-F19 = C29-F20 = C29-F21 = C29-F19' = C29-F20' = C29-F21'
 1.36 with sigma of 0.01
 C37-C38 = C38-C39 = C39-C40 = C40-C41 = C41-C42 = C42-C43
 1.54 with sigma of 0.01
 C37-C39 = C38-C40 = C39-C41 = C40-C42 = C41-C43
 2.5 with sigma of 0.02
3. Rigid bond restraints
 O12, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
F19 \\sim F20 \\sim F21 \\sim F19' \\sim F20' \\sim F21': within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02
F22 \\sim F23 \\sim F24 \\sim F22' \\sim F23' \\sim F24': within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F22) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F22')
\\sim Ueq, Uanis(F23') \\sim Ueq, Uanis(F24') \\sim Ueq, Uanis(F1) \\sim Ueq,
Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F1') \\sim Ueq, Uanis(F2')
\\sim Ueq, Uanis(F3') \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq,
Uanis(F6) \\sim Ueq, Uanis(F4') \\sim Ueq, Uanis(F5') \\sim Ueq, Uanis(F6')
\\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq,
Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F13)
\\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F16) \\sim Ueq,
Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F20)
\\sim Ueq, Uanis(F21) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(F20') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: F1(0.5) F2(0.5) F3(0.5) F1'(0.5) F2'(0.5) F3'(0.5) F4(0.5) F5(0.5)
 F6(0.5) F4'(0.5) F5'(0.5) F6'(0.5) F19(0.5) F20(0.5) F21(0.5) F22(0.5)
 F23(0.5) F24(0.5) F19'(0.5) F20'(0.5) F21'(0.5) F22'(0.5) F23'(0.5) F24'(0.5)
 C37(0.5) C38(0.5) C39(0.5) C40(0.5) C41(0.5) C42(0.5) C43(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C16(H16), C21(H21),
 C26(H26), C31(H31), C34(H34)
6.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
6.c Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              73386
_shelx_hkl_checksum              24056
_olex2_submission_special_instructions 'No special instructions were received'