Cobalt Clusters with Cubane-Type Topologies Based on Trivacant Polyoxometalate Ligands.
Duan, Yan; Clemente-Juan, Juan M; Giménez-Saiz, Carlos; Coronado, Eugenio; Inorganic chemistry 55 (2016) 925–938; doi:10.1021/acs.inorgchem.5b02532

data_4344607
_publ_section_title
;
 Cobalt Clusters with Cubane-Type Topologies Based on Trivacant
 Polyoxometalate Ligands.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              925
_journal_page_last               938
_journal_paper_doi               10.1021/acs.inorgchem.5b02532
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'Co4 Cs2.5 H33 Na1.5 O52 P W9'
_chemical_formula_weight         3153.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.7139(2)
_cell_length_b                   21.6677(2)
_cell_length_c                   20.02760(10)
_cell_measurement_reflns_used    143954
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     10724.65(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      292(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1097
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            95392
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    22.243
_exptl_absorpt_correction_T_max  0.286
_exptl_absorpt_correction_T_min  0.184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            red-violet
_exptl_crystal_density_diffrn    3.906
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             11136
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The structure contains channels parallel to the crystallographic c axis containing 
disordered water molecules and sodium cations which could not be modelled as discrete 
atomic sites. We employed PLATON SQUEEZE to calculate the contribution to the diffraction 
from the solvent/cation region and thereby produced a set of solvent-free diffraction 
intensities. The final formula was calculated from the TGA combined with elemental 
analysis data, which indicated that 1.5 sodium cations and 5.0 additional water 
molecules had to be added to the formula of the polyoxometalate.
;
_refine_diff_density_max         4.189
_refine_diff_density_min         -3.013
_refine_diff_density_rms         0.644
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         12274
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0899P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1481
_reflns_number_gt                8943
_reflns_number_total             12274
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02532_si_001.cif
_cod_data_source_block           Na1.5Cs2.5-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_formula_sum        'Co4 Cs2.50 H33 Na1.50 O52 P W9'
_cod_database_code               4344607