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_7702251
_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         'C62 H82 N6 O24 Tm4, 2(C H4 O)'
_chemical_formula_sum            'C64 H90 N6 O26 Tm4'
_chemical_formula_weight         2035.13
_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             2019-08-23
_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                 99.221(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.8499(11)
_cell_length_b                   15.0852(12)
_cell_length_c                   17.2237(13)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.39
_cell_volume                     3808.5(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0853
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            64590
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.431
_diffrn_reflns_theta_min         2.392
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.692
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0785 before and 0.0650 after correction.
The Ratio of minimum to maximum transmission is 0.3913.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.752
_refine_diff_density_min         -1.892
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         7817
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0915P)^2^+27.9360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1439
_refine_ls_wR_factor_ref         0.1812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5173
_reflns_number_total             7817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03478a2.cif
_cod_data_source_block           8
_cod_database_code               7702251
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.540
_shelx_estimated_absorpt_t_min   0.315
_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
 O10-H10
 0.87 with sigma of 0.01
 O11-H11
 0.87 with sigma of 0.01
 O12-H12
 0.87 with sigma of 0.01
 H13-H32B
 2.15 with sigma of 0.02
 O9-H13
 2.1 with sigma of 0.02
 C31-H10
 1.929942 with sigma of 0.02
 Tm2-H10
 3.011078 with sigma of 0.02
 C29-H11
 1.905868 with sigma of 0.02
 Tm1-H11
 3.113542 with sigma of 0.02
 C30-H12
 1.901591 with sigma of 0.02
 Tm1-H12
 3.145765 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C21(H21), C3(H3), C9(H9), C4(H4), C7(H7), C10(H10A), C2(H2),
 C26(H26), C1(H1), C11(H11A)
3.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C29(H29A,H29B,
 H29C), C28(H28A,H28B,H28C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C18(H18A,
 H18B,H18C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C)
3.c Idealised tetrahedral OH refined as rotating group:
 O13(H13)
;
_shelx_res_checksum              38907
_olex2_submission_special_instructions 'No special instructions were received'