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_7702250
_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         'C56 H62 Lu4 N6 O20, 2(C H2 Cl2)'
_chemical_formula_sum            'C58 H66 Cl4 Lu4 N6 O20'
_chemical_formula_weight         2008.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-07-17
_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                96.775(2)
_cell_angle_beta                 94.875(2)
_cell_angle_gamma                101.833(2)
_cell_formula_units_Z            1
_cell_length_a                   8.5600(4)
_cell_length_b                   14.0982(7)
_cell_length_c                   14.3191(6)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.44
_cell_measurement_theta_min      2.21
_cell_volume                     1668.88(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      150.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0453
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31259
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.445
_diffrn_reflns_theta_min         2.213
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.099
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1093 before and 0.0585 after correction.
The Ratio of minimum to maximum transmission is 0.6150.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.999
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.968
_refine_diff_density_min         -1.190
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6865
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0157P)^2^+12.2094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5844
_reflns_number_total             6865
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03478a2.cif
_cod_data_source_block           10
_cod_original_cell_volume        1668.87(13)
_cod_database_code               7702250
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.482
_shelx_estimated_absorpt_t_min   0.334
_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, All O(H,H) groups
2. Restrained distances
 H10B_$1-H7_$2
 2.2 with sigma of 0.02
3.a Rotating group:
 O10(H10A,H10B)
3.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B)
3.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C4(H4), C7(H7), C11(H11), C21(H21), C9(H9), C26(H26), C3(H3),
 C1(H1), C10(H10), C2(H2)
3.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C18(H18A,H18B,H18C), C14(H14A,H14B,H14C), C19(H19A,H19B,
 H19C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              50238
_olex2_submission_special_instructions 'No special instructions were received'