Linear-shaped Ln and Ln clusters constructed by a polydentate Schiff base ligand and a β-diketone co-ligand: structures, fluorescence properties, magnetic refrigeration and single-molecule magnet behavior.
Wang, Wen-Min; He, Li-Yuan; Wang, Xin-Xin; Shi, Ying; Wu, Zhi-Lei; Cui, Jian-Zhong; Dalton transactions (Cambridge, England : 2003) 48 (2019) 16744–16755; doi:10.1039/c9dt03478a

data_7702254
_publ_section_title
;
 Linear-shaped Ln and Ln clusters constructed by a polydentate Schiff base
 ligand and a \b-diketone co-ligand: structures, fluorescence properties,
 magnetic refrigeration and single-molecule magnet behavior.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16744
_journal_page_last               16755
_journal_paper_doi               10.1039/c9dt03478a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C60 H74 N6 O22 Tb4, C H4 O'
_chemical_formula_sum            'C61 H78 N6 O23 Tb4'
_chemical_formula_weight         1898.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-25 deposited with the CCDC.	2019-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.671(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3614(16)
_cell_length_b                   12.8302(13)
_cell_length_c                   35.007(4)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.32
_cell_volume                     6876.6(13)
_computing_cell_refinement       '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)'
_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 0.963
_diffrn_measured_fraction_theta_max 0.966
_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  0.1138
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            127695
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.284
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.143
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1075 before and 0.0803 after correction.
The Ratio of minimum to maximum transmission is 0.7946.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_description       block
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         4.653
_refine_diff_density_min         -2.965
_refine_diff_density_rms         0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         13069
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1548
_refine_ls_R_factor_gt           0.0944
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+550.1950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2244
_refine_ls_wR_factor_ref         0.2606
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8236
_reflns_number_total             13069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03478a2.cif
_cod_data_source_block           5
_cod_original_cell_volume        6876.5(12)
_cod_database_code               7702254
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.595
_shelx_estimated_absorpt_t_min   0.412
_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
 O19-H19
 0.87 with sigma of 0.01
 O20-H20A
 0.87 with sigma of 0.01
 O21-H21
 0.87 with sigma of 0.01
 O22-H22
 0.87 with sigma of 0.01
 C57-H19
 1.93977 with sigma of 0.02
 Tb4-H19
 3.066695 with sigma of 0.02
 C58-H20A
 1.928834 with sigma of 0.02
 Tb3-H20A
 3.011072 with sigma of 0.02
 C59-H21
 1.871392 with sigma of 0.02
 Tb2-H21
 2.998326 with sigma of 0.02
 C60-H22
 1.943787 with sigma of 0.02
 Tb1-H22
 2.978219 with sigma of 0.02
3. Rigid bond restraints
 N6, C20, C21
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C56, C55
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C24(H24), C23(H23), C22(H22A), C4(H4), C3(H3), C2(H2), C1(H1),
 C11(H11), C10(H10), C9(H9), C7(H7), C44(H44), C29(H29), C17(H17), C16(H16),
 C15(H15), C14(H14), C34(H34), C49(H49), C39(H39), C54(H54)
5.b Fitted hexagon refined as free rotating group:
 C26(C25,C24,C23,C22,C21), N1(C5,C4,C3,C2,C1), C13(C12,C11,C10,C9,C8), N4(C18,
 C17,C16,C15,C14)
5.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C59(H59A,H59B,H59C), C58(H58A,H58B,H58C), C36(H36A,H36B,
 H36C), C51(H51A,H51B,H51C), C47(H47A,H47B,H47C), C41(H41A,H41B,H41C), C37(H37A,
 H37B,H37C), C42(H42A,H42B,H42C), C57(H57A,H57B,H57C), C56(H56A,H56B,H56C),
 C27(H27A,H27B,H27C), C32(H32A,H32B,H32C), C61(H61A,H61B,H61C), C31(H31A,H31B,
 H31C), C52(H52A,H52B,H52C), C60(H60A,H60B,H60C)
5.d Idealised tetrahedral OH refined as rotating group:
 O23(H23A)
;
_shelx_res_checksum              13738
_olex2_submission_special_instructions 'No special instructions were received'