Rationally assembled nonanuclear lanthanide clusters: Dy9 displays slow relaxation of magnetization and Tb9 serves as luminescent sensor for Fe3+, CrO42- and Cr2O72-
Huang, Yuan; Qin, Yaru; Ge, Yu; Cui, Yanfeng; Zhang, Xiamei; Li, Yahong; Yao, Jinlei; New Journal of Chemistry 43 (2019) 19344–19354; doi:10.1039/C9NJ04893F

data_7059032
_publ_section_title
;
 Rationally assembled nonanuclear lanthanide clusters: Dy9 displays slow
 relaxation of magnetization and Tb9 serves as luminescent sensor for
 Fe3+, CrO42- and Cr2O72-
;
_journal_issue                   48
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19344
_journal_page_last               19354
_journal_paper_doi               10.1039/C9NJ04893F
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C144 H168 Eu9 N16 O42, H3 O, H2O'
_chemical_formula_sum            'C144 H173 Eu9 N16 O44'
_chemical_formula_weight         4206.47
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-06 deposited with the CCDC.	2019-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.6995(3)
_cell_length_b                   21.6995(3)
_cell_length_c                   17.9503(7)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.46
_cell_volume                     8452.2(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_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  0.0740
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24961
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_min         2.629
_exptl_absorpt_coefficient_mu    3.361
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.2085 before and 0.0688 after correction.
The Ratio of minimum to maximum transmission is 0.3580.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       block
_exptl_crystal_F_000             4094
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.189
_refine_diff_density_min         -1.776
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8031
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0758
_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^)+308.0675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5844
_reflns_number_total             8031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04893f2.cif
_cod_data_source_block           t_sq_s
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7059032
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 O3, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Riding coordinates:
 O8(H8), O10(H10)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C32(H32A,H32B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8A), C10(H10A), C13(H13), C14(H14), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C24(H24), C30(H30), C31(H31), C34(H34),
  C35(H35), C36(H36)
4.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              39110
_shelx_fab_checksum              60068
_olex2_submission_special_instructions 'No special instructions were received'