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_7702247
_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 Dy4 N6 O24, 2(C H4 O)'
_chemical_formula_sum            'C64 H90 Dy4 N6 O26'
_chemical_formula_weight         2009.41
_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             2018-04-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-08-25 deposited with the CCDC.	2019-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.366(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.8441(11)
_cell_length_b                   15.0331(10)
_cell_length_c                   17.0783(13)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.42
_cell_volume                     3760.3(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      293(2)
_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  0.0890
_diffrn_reflns_av_unetI/netI     0.0525
_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            50379
_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         26.414
_diffrn_reflns_theta_min         2.164
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.008
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0831 before and 0.0639 after correction.
The Ratio of minimum to maximum transmission is 0.9184.
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             1976
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.164
_refine_diff_density_min         -1.950
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         7707
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0620P)^2^+10.3780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1269
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5427
_reflns_number_total             7707
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03478a2.cif
_cod_data_source_block           6
_cod_database_code               7702247
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.667
_shelx_estimated_absorpt_t_min   0.422
_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-H
 0.85 with sigma of 0.01
 O11-HA
 0.85 with sigma of 0.01
 O12-HB
 0.85 with sigma of 0.01
 H13-H32B
 2.2 with sigma of 0.02
 H13-O7
 1.9 with sigma of 0.02
 H13-H32C
 2.2 with sigma of 0.02
 C29-H
 1.911813 with sigma of 0.02
 Dy2-H
 2.962091 with sigma of 0.02
 C30-HA
 1.902807 with sigma of 0.02
 Dy1-HA
 3.083618 with sigma of 0.02
 C31-HB
 1.887822 with sigma of 0.02
 Dy1-HB
 3.072461 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C4(HX), C12(H1AA), C11(H2AA), C2(H6AA), C13(H7AA), C21(H8AA), C16(H9AA),
 C10(H0BA), C7(H1BA), C3(H2BA), C26(H3BA)
4.b Idealised Me refined as rotating group:
 C18(HC,HD,HE), C14(HF,HG,HH), C23(HI,HJ,HK), C24(HL,HM,HN), C28(HO,HP,HQ),
 C31(HR,HS,HT), C30(HU,HV,HW), C19(HY,HZ,H0AA), C29(H3AA,H4AA,H5AA), C32(H32A,
 H32B,H32C)
4.c Idealised tetrahedral OH refined as rotating group:
 O13(H13)
;
_shelx_res_checksum              7933
_olex2_submission_special_instructions 'No special instructions were received'