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_7702246
_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         'C64 H90 N6 Nd4 O26, 2(C H4 O)'
_chemical_formula_sum            'C66 H98 N6 Nd4 O28'
_chemical_formula_weight         2000.46
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-05-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2019-08-25 deposited with the CCDC.	2019-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   47.810(3)
_cell_length_b                   47.810(3)
_cell_length_c                   9.5696(6)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.34
_cell_volume                     18944(2)
_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)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0668
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            73132
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.016
_diffrn_reflns_theta_min         2.184
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.501
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1132 before and 0.0685 after correction.
The Ratio of minimum to maximum transmission is 0.7360.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       block
_exptl_crystal_F_000             9000
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.713
_refine_diff_density_min         -1.278
_refine_diff_density_rms         0.160
_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     493
_refine_ls_number_reflns         8287
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0521P)^2^+221.5431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6592
_reflns_number_total             8287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03478a2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7702246
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.721
_shelx_estimated_absorpt_t_min   0.531
_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) groups
2. Restrained distances
 O13-H13
 0.87 with sigma of 0.01
 O12-H12
 0.87 with sigma of 0.01
 O11-H11
 0.87 with sigma of 0.01
 O10-H10
 0.87 with sigma of 0.01
 N2-H14
 2.2 with sigma of 0.02
 C32-H13
 1.927127 with sigma of 0.02
 Nd1-H13
 3.102604 with sigma of 0.02
 C31-H12
 1.941813 with sigma of 0.02
 Nd2-H12
 3.186771 with sigma of 0.02
 C30-H11
 1.935613 with sigma of 0.02
 Nd1-H11
 3.357953 with sigma of 0.02
 C29-H10
 1.908648 with sigma of 0.02
 Nd2-H10
 3.062567 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C16(H16), C4(H4), C11(H11A), C1(H1), C10(H10A), C2(H2), C3(H3), C9(H9)
3.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C), C14(H14A,H14B,
 H14C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C18(H18A,H18B,H18C), C32(H32A,
 H32B,H32C), C19(H19A,H19B,H19C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C)
3.d Idealised tetrahedral OH refined as rotating group:
 O14(H14)
;
_shelx_res_checksum              5039
_shelx_fab_checksum              44580
_olex2_submission_special_instructions 'No special instructions were received'