Butterfly-shaped tetranuclear Ln4 clusters showing magnetic refrigeration and single molecule-magnet behavior
Wang, Wen-Min; Han, Tong-Lei; Shao, Yan-Ling; Qiao, Xin-Yi; Wu, Zhi-Lei; Wang, Qing-Li; Shi, Peng Fei; Gao, Hong-Ling; Cui, Jian-Zhong; New Journal of Chemistry 42 (2018) 14949–; doi:10.1039/C8NJ02479K

data_7057605
_publ_section_title
;
 Butterfly-shaped tetranuclear Ln4 clusters showing magnetic refrigeration
 and single molecule-magnet behavior
;
_journal_issue                   18
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14949
_journal_paper_doi               10.1039/C8NJ02479K
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C152 H120 Dy4 N12 O16'
_chemical_formula_sum            'C152 H120 Dy4 N12 O16'
_chemical_formula_weight         3020.59
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-27 deposited with the CCDC.
2018-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.505(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.813(4)
_cell_length_b                   21.610(5)
_cell_length_c                   18.034(5)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.94
_cell_volume                     6544(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_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)'
_diffrn_ambient_temperature      299.24
_diffrn_measured_fraction_theta_full 0.993
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47161
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.939
_exptl_absorpt_coefficient_mu    2.328
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1018 before and 0.0598 after correction.
The Ratio of minimum to maximum transmission is 0.7699.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       block
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.677
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         11466
_refine_ls_number_restraints     358
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1431
_refine_ls_R_factor_gt           0.0817
_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^)+(0.0773P)^2^+83.1927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1876
_refine_ls_wR_factor_ref         0.2350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6803
_reflns_number_total             11466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj02479k2.cif
_cod_data_source_block           111_sq
_cod_depositor_comments
'Adding full bibliography for 7057603--7057605.cif.'
_cod_database_code               7057605
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.784
_shelx_estimated_absorpt_t_min   0.464
_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
2. Restrained distances
 O8-H8
 0.85 with sigma of 0.02
 H49A_$1-H24_$2
 2.2 with sigma of 0.02
 H8_$3-O6
 2.2 with sigma of 0.02
 C48A-C48 \\sim C48-C48B
 with sigma of 0.02
3. Rigid bond restraints
 C46B, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C14, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C4, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C48B, C48A, C48
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C55, C56
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C33 \\sim C32 \\sim C31: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C30 \\sim C29 \\sim C34: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C2 \\sim C3 \\sim C4 \\sim C5: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C4 \\sim C7: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C48 \\sim C48B \\sim C48A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C56 \\sim C55: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C25 \\sim C26 \\sim C27: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C45 \\sim C46A \\sim C46B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C25 \\sim C23 \\sim C24: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C12) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C5)
\\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C57) \\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C48A) \\sim Ueq, Uanis(C49B) \\sim Ueq, Uanis(C47B) \\sim Ueq,
Uanis(C46B) \\sim Ueq, Uanis(C48B) \\sim Ueq, Uanis(C46A) \\sim Ueq,
Uanis(C47A) \\sim Ueq, Uanis(C49A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C30) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C31) \\sim Ueq,
Uanis(C53) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C55)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C27) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C47B) = Uanis(C46B) = Uanis(C46A) = Uanis(C47A) = Uanis(C48A) =
Uanis(C49B) = Uanis(C48B) = Uanis(C49A)
5. Others
 Sof(C48A)=Sof(H48A)=Sof(H45A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=Sof(H47A)=
 Sof(C49A)=Sof(H49A)=1-FVAR(1)
 Sof(C49B)=Sof(H49B)=Sof(C47B)=Sof(H47B)=Sof(H45)=Sof(C46B)=Sof(H46B)=
 Sof(C48B)=Sof(H48B)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C37(H37), C38(H38), C15(H15), C16(H16), C43(H43), C69(H69), C44(H44),
 C13(H13), C42(H42), C20(H20), C60(H60), C59(H59), C22(H22), C21(H21), C66(H66),
  C64(H64), C12(H12), C8(H8A), C9(H9), C11(H11), C65(H65), C57(H57), C5(H5),
 C6(H6), C1(H1), C2(H2), C3(H3), C74(H74), C27(H27), C28(H28), C23(H23),
 C24(H24), C25(H25), C53(H53), C52(H52), C56(H56), C55(H55), C35(H35), C31(H31),
  C30(H30), C34(H34), C33(H33), C48A(H48A), C49B(H49B), C47B(H47B), C45(H45),
 C45(H45A), C46B(H46B), C48B(H48B), C46A(H46A), C47A(H47A), C49A(H49A)
6.b Fitted hexagon refined as free rotating group:
 C39(C40,C41,C36,C37,C38), C17(C18,C19,C14,C15,C16), C61(C60,C59,C58,C63,C62),
 C12(C7,C8,C9,C10,C11), C5(C6,C1,C2,C3,C4), C26(C27,C28,C23,C24,C25), C54(C53,
 C52,C51,C56,C55), C32(C31,C30,C29,C34,C33)
6.c Idealised Me refined as rotating group:
 C71(H71A,H71B,H71C), C67(H67A,H67B,H67C), C72(H72A,H72B,H72C), C76(H76A,H76B,
 H76C)
;
_shelx_res_checksum              54898
_shelx_fab_checksum              54927
_olex2_submission_special_instructions 'No special instructions were received'