Utilizing the Adaptive Polyoxometalate [As2W19O67(H2O)]14- To Support a Polynuclear Lanthanoid-Based Single-Molecule Magnet
Chris Ritchie; Manfred Speldrich; Robert W. Gable; Lorenzo Sorace; Paul Kögerler; Colette Boskovic; Inorganic Chemistry 50 (2011) 7004–7014; doi:10.1021/ic200366a

data_4325756
_publ_contact_author_address
'School of Chemistry, University of Melbourne, Victoria, 3010, Australia'
_publ_contact_author_email       c.boskovic@unimelb.edu.au
_publ_contact_author_name        'Dr Colette Boskovic'
_publ_contact_author_phone       +61-3-8344-4971
_publ_section_title
;
 Utilizing the Adaptive Polyoxometalate [As2W19O67(H2O)]14- To Support a
 Polynuclear Lanthanoid-Based Single-Molecule Magnet
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7004
_journal_page_last               7014
_journal_paper_doi               10.1021/ic200366a
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety
'(C6 H13 N2)8, Li8, (H35 Dy4 As5 W40 O158 C4 N2),25(H2 O)'
_chemical_formula_sum            'C52 H189 As5 Dy4 Li8 N18 O183 W40'
_chemical_formula_weight         12429.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.349(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.7245(7)
_cell_length_b                   25.1124(5)
_cell_length_c                   35.1823(10)
_cell_measurement_reflns_used    7825
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      40.5183
_cell_measurement_theta_min      2.6691
_cell_volume                     23794.6(11)
_computing_cell_refinement
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) 
(compiled Jan 10 2008,16:37:18) 
;
_computing_data_collection
; 
CrysAlis CCD, Oxford Diffraction Ltd., 
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) 
(compiled Jan 10 2008,16:37:18) 
;
_computing_data_reduction
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) 
(compiled Jan 10 2008,16:37:18) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.0711
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'XCalibur S CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0672
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19828
_diffrn_reflns_theta_full        40.61
_diffrn_reflns_theta_max         40.61
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    42.915
_exptl_absorpt_correction_T_max  0.076
_exptl_absorpt_correction_T_min  0.034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) 
(compiled Jan 10 2008,16:37:18) 
empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.470
_exptl_crystal_description       needle
_exptl_crystal_F_000             22016
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.571
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         7299
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                5312
_reflns_number_total             7299
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic200366a_si_002_3.cif
_cod_data_source_block           Compound3Dy
_cod_original_cell_volume        23794.6(10)
_cod_original_sg_symbol_Hall     '-C 2yc '
_cod_database_code               4325756