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_7057604
_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 H122 Gd4 N12 O16, 2(C2 H3 N)'
_chemical_formula_sum            'C156 H128 Gd4 N14 O16'
_chemical_formula_weight         3083.72
_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   geom
_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                 110.487(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.845(4)
_cell_length_b                   21.607(7)
_cell_length_c                   18.168(4)
_cell_measurement_reflns_used    13986
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     6562(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b42'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b42'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133.15
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0466
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_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            70495
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.018
_diffrn_reflns_theta_max         25.018
_diffrn_reflns_theta_min         3.043
_exptl_absorpt_coefficient_mu    2.068
_exptl_absorpt_correction_T_max  0.7605
_exptl_absorpt_correction_T_min  0.6825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3092
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.828
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         11565
_refine_ls_number_restraints     275
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0589P)^2^+15.8019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9639
_reflns_number_total             11565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj02479k2.cif
_cod_data_source_block           m20170329c1
_cod_depositor_comments
'Adding full bibliography for 7057603--7057605.cif.'
_cod_original_cell_volume        6563(3)
_cod_database_code               7057604
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.682
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N7-C77
 1.12 with sigma of 0.01
 C77-C78
 1.54 with sigma of 0.01
 N7-C78
 2.66 with sigma of 0.02
 C14-C17 = C14-C17'
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C21 \\sim C22 \\sim C17'
\\sim C18' \\sim C19' \\sim C20' \\sim C21' \\sim C21' \\sim C22': within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C77) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(N7) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq,
Uanis(C17') \\sim Ueq, Uanis(C18') \\sim Ueq, Uanis(C19') \\sim Ueq,
Uanis(C20') \\sim Ueq, Uanis(C21') \\sim Ueq, Uanis(C21') \\sim Ueq,
Uanis(C22') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C17(0.5) C18(0.5) H18(0.5) C19(0.5) H19(0.5) C20(0.5) H20(0.5)
 C21(0.5) H21(0.5) C22(0.5) H22(0.5) C17'(0.5) C18'(0.5) H18'(0.5) C19'(0.5)
 H19'(0.5) C20'(0.5) H20'(0.5) C21'(0.5) H21'(0.5) C22'(0.5) H22'(0.5)
5.a Ternary CH refined with riding coordinates:
 O8(H8)
5.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C3(H3), C4(H4A), C7(H7), C8(H8A), C9(H9), C10(H10), C12(H12),
 C13(H13), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
  C18'(H18'), C19'(H19'), C20'(H20'), C21'(H21'), C22'(H22'), C25(H25),
 C26(H26), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C37(H37),
  C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C47(H47),
 C48(H48), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C59(H59),
  C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C69(H69), C74(H74)
5.c Fitted hexagon refined as free rotating group:
 C17'(C18',C19',C20',C21',C22')
5.d Idealised Me refined as rotating group:
 C67(H67A,H67B,H67C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C76(H76A,H76B,
 H76C), C78(H78A,H78B,H78C)
;
_shelx_res_checksum              29014
_olex2_submission_special_instructions 'No special instructions were received'