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_7702249
_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 Sm4, 2(C H4 O)'
_chemical_formula_sum            'C64 H90 N6 O26 Sm4'
_chemical_formula_weight         1960.81
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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                 98.526(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.4789(12)
_cell_length_b                   15.0651(7)
_cell_length_c                   20.8613(11)
_cell_measurement_reflns_used    9180
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.39
_cell_volume                     7608.1(7)
_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 0.999
_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  0.0744
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            105509
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.465
_diffrn_reflns_theta_min         2.258
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.121
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0926 before and 0.0652 after correction.
The Ratio of minimum to maximum transmission is 0.7015.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       block
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.973
_refine_diff_density_min         -1.610
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     941
_refine_ls_number_reflns         15644
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+37.7850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1358
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11350
_reflns_number_total             15644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03478a2.cif
_cod_data_source_block           2
_cod_database_code               7702249
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.687
_shelx_estimated_absorpt_t_min   0.498
_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
 O22-H22
 0.87 with sigma of 0.01
 O19-H19
 0.87 with sigma of 0.01
 O20-H20
 0.87 with sigma of 0.01
 O24-H24
 0.87 with sigma of 0.01
 O23-H23
 0.87 with sigma of 0.01
 O21-H21
 0.87 with sigma of 0.01
 C60-H22
 1.924193 with sigma of 0.02
 Sm11-H22
 3.023928 with sigma of 0.02
 C57-H19
 1.897206 with sigma of 0.02
 Sm15-H19
 3.027236 with sigma of 0.02
 C58-H20
 1.899104 with sigma of 0.02
 Sm6-H20
 3.107701 with sigma of 0.02
 C62-H24
 1.910975 with sigma of 0.02
 Sm6-H24
 3.156604 with sigma of 0.02
 C61-H23
 1.90893 with sigma of 0.02
 Sm2-H23
 3.118373 with sigma of 0.02
 C59-H21
 1.899432 with sigma of 0.02
 Sm2-H21
 3.147849 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C54(H54), C2(H2), C1(H1), C39(H39), C16(H16), C15(H15), C9(H9), C10(H10),
 C22(H22A), C49(H49), C3(H3), C23(H23A), C4(H4), C7(H7), C20(H20A), C17(H17),
 C14(H14), C29(H29), C11(H11), C44(H44), C24(H24A), C34(H34)
3.b Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C37(H37A,H37B,H37C), C59(H59A,H59B,H59C), C58(H58A,H58B,
 H58C), C31(H31A,H31B,H31C), C36(H36A,H36B,H36C), C51(H51A,H51B,H51C), C62(H62A,
 H62B,H62C), C64(H64A,H64B,H64C), C56(H56A,H56B,H56C), C42(H42A,H42B,H42C),
 C27(H27A,H27B,H27C), C46(H46A,H46B,H46C), C60(H60A,H60B,H60C), C61(H61A,H61B,
 H61C), C63(H63A,H63B,H63C), C32(H32A,H32B,H32C), C57(H57A,H57B,H57C), C41(H41A,
 H41B,H41C), C47(H47A,H47B,H47C)
3.c Idealised tetrahedral OH refined as rotating group:
 O26(H26), O25(H25)
;
_shelx_res_checksum              64923
_olex2_submission_special_instructions 'No special instructions were received'