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_7059034
_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 Ho9 N16 O42, H3 O, 2(H2O)'
_chemical_formula_sum            'C144 H175 Ho9 N16 O45'
_chemical_formula_weight         4332.56
_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             2019-11-06
_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                   21.6913(4)
_cell_length_b                   21.6913(4)
_cell_length_c                   17.8971(7)
_cell_measurement_reflns_used    8558
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9450
_cell_measurement_theta_min      3.1760
_cell_volume                     8420.8(4)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.1107
_diffrn_reflns_av_unetI/netI     0.1493
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37511
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         3.039
_exptl_absorpt_coefficient_mu    4.250
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54908
_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    1.688
_exptl_crystal_description       block
_exptl_crystal_F_000             4166
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.564
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.827
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7747
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      0.834
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0548
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1131
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4686
_reflns_number_total             7747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04893f2.cif
_cod_data_source_block           t2_sq
_cod_original_cell_volume        8420.8(5)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7059034
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C35, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O8, C36, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O8, C36, C35, N1, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C35 \\sim C36 \\sim C34: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O8 \\sim C36 \\sim N1: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O8 \\sim C36 \\sim N1 \\sim C35 \\sim C34: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C36) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(N1)
\\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Rigid body (RIGU) restrains
 C36, C34, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O8, C36, C35, N1, C34
 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:
 C7(H7A,H7B), C24(H24A,H24B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11A), C13(H13),
 C18(H18), C19(H19), C22(H22), C23(H23), C26(H26), C27(H27), C28(H28), C29(H29),
  C33(H33), C36(H36)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              99182
_shelx_fab_checksum              1527
_olex2_submission_special_instructions 'No special instructions were received'