A wheel-shaped Dy(III) single-molecule magnet supported by polyoxotungstates
Huo, Yu; Chen, Yan-Cong; Liu, Jun-Liang; Jia, Jian-Hua; Chen, Wen-Bin; Wu, Si-Guo; Tong, Mingliang; Dalton Transactions  (2017) –; doi:10.1039/C7DT03721J

data_7044725
_publ_section_title
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 A wheel-shaped Dy(III) single-molecule magnet supported by
 polyoxotungstates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03721J
_journal_year                    2017
_chemical_formula_moiety         'As6 Cs15 Dy6 K9 Na12 O263 W54, 18(O)'
_chemical_formula_sum            'As6 Cs15 Dy6 H166 K9 Na12 O281 W54'
_chemical_formula_weight         18637.17
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   23.4503(8)
_cell_length_b                   23.4503(8)
_cell_length_c                   14.6472(5)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.44
_cell_volume                     6975.6(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      120.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_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  0.0603
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38526
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.550
_diffrn_reflns_theta_min         2.441
_exptl_absorpt_coefficient_mu    26.649
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0753 before and 0.0548 after correction.
The Ratio of minimum to maximum transmission is 0.7712.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.437
_exptl_crystal_description       block
_exptl_crystal_F_000             8132
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.209
_refine_diff_density_min         -2.993
_refine_diff_density_rms         0.492
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         10676
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0592P)^2^+246.2228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7288
_reflns_number_total             10676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03721j1.cif
_cod_data_source_block           a
_cod_original_cell_volume        6975.6(5)
_cod_database_code               7044725
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.349
_shelx_estimated_absorpt_t_min   0.176
_olex2_refinement_description
;
1. Shared sites
{K2, O18W}
2. Uiso/Uaniso restraints and constraints
Uanis(O26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(K5) \\sim Ueq, Uanis(O5W) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(K2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(K2) = Uanis(O18W)
3. Others
 Fixed Sof: O10W(0.5) O13W(0.5) O14W(0.5) O15W(0.5) O16W(0.5) Cs1(0.5) K2(0.5)
 K5(0.33333) K3(0.5) O18W(0.5) O12W(0.5) O5W(0.66667)
;
_shelx_res_checksum              60776
_shelx_hkl_checksum              96113
_olex2_submission_special_instructions 'No special instructions were received'