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_7059033
_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 N16 O42 Tb9, H3 O, 3(H2O)'
_chemical_formula_sum            'C144 H177 N16 O46 Tb9'
_chemical_formula_weight         4296.52
_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
_audit_creation_date             2019-10-31
_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                   21.5916(3)
_cell_length_b                   21.5916(3)
_cell_length_c                   17.8737(4)
_cell_measurement_reflns_used    12737
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6590
_cell_measurement_theta_min      3.1210
_cell_volume                     8332.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32014
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.678
_diffrn_reflns_theta_min         3.106
_exptl_absorpt_coefficient_mu    3.841
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_description       block
_exptl_crystal_F_000             4130
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.043
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7897
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0268P)^2^+66.3568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6183
_reflns_number_total             7897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04893f2.cif
_cod_data_source_block           t9_sq
_cod_original_cell_volume        8332.7(3)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7059033
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.802
_shelx_estimated_absorpt_t_min   0.514
_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
2. Rigid bond restraints
 C34, N4, O10, C35, C36
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C34 \\sim N4 \\sim O10 \\sim C35 \\sim C36: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.001
Uanis(C34) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Rigid body (RIGU) restrains
 C34, N4, O10, C35, C36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C8(H8), C9(H9), C10(H10), C13(H13), C15(H15), C16(H16),
 C18(H18), C19(H19), C20(H20), C22(H22), C25(H25), C26(H26), C29(H29), C30(H30),
  C31(H31), C34(H34)
5.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              25672
_shelx_fab_checksum              1779
_olex2_submission_special_instructions 'No special instructions were received'