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_7702248
_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 Gd4 N6 O24'
_chemical_formula_sum            'C62 H82 Gd4 N6 O24'
_chemical_formula_weight         1924.33
_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                 99.430(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.8527(7)
_cell_length_b                   15.0504(8)
_cell_length_c                   17.1650(7)
_cell_measurement_reflns_used    9666
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.355
_cell_measurement_theta_min      2.780
_cell_volume                     3785.2(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_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            46971
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.420
_diffrn_reflns_theta_min         2.400
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.533
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1144 before and 0.0674 after correction.
The Ratio of minimum to maximum transmission is 0.7721.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       block
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         6.178
_refine_diff_density_min         -2.549
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7734
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1243P)^2^+46.6535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1823
_refine_ls_wR_factor_ref         0.2081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5772
_reflns_number_total             7734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03478a2.cif
_cod_data_source_block           4
_cod_database_code               7702248
_shelx_shelxl_version_number     2016/6
_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
 O11-H11
 0.87 with sigma of 0.01
 O10-H10
 0.87 with sigma of 0.01
 O12-H12
 0.87 with sigma of 0.01
 O3_$1-H12
 2.3 with sigma of 0.02
 C30-H11
 1.906973 with sigma of 0.02
 Gd2-H11
 3.112809 with sigma of 0.02
 C29-H10
 1.930313 with sigma of 0.02
 Gd1-H10
 3.001292 with sigma of 0.02
 C31-H12
 1.907907 with sigma of 0.02
 Gd2-H12
 3.091905 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C7(H7), C12(H12A), C2(H2), C4(H4), C3(H3), C21(H21), C26(H26),
 C1(H1), C16(H16), C11(H11A)
3.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C28(H28A,H28B,
 H28C), C23(H23A,H23B,H23C), C14(H14A,H14B,H14C), C19(H19A,H19B,H19C), C24(H24A,
 H24B,H24C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              55701
_olex2_submission_special_instructions 'No special instructions were received'