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_4344609
_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            'Co8 H58 K5 Na2 O100 P2 W18'
_chemical_formula_weight         5742.62
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.041(3)
_cell_angle_beta                 83.369(3)
_cell_angle_gamma                73.088(3)
_cell_formula_units_Z            1
_cell_length_a                   10.2222(3)
_cell_length_b                   12.6115(4)
_cell_length_c                   17.8646(6)
_cell_measurement_reflns_used    10644
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      27.9860
_cell_measurement_theta_min      3.1780
_cell_volume                     2144.21(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_details
;
  1 omega  -88.00   12.00   0.8000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7276  -77.0000   60.0000 125

  2 omega  -75.00   -3.00   0.8000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7276  125.0000  -78.0000 90

  3 omega  -94.00  -35.60   0.8000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7276 -178.0000  -30.0000 73

  4 omega  -20.00   60.00   0.8000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3526  -99.0000  -90.0000 100

  5 omega   -3.00   86.60   0.8000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3526   57.0000 -180.0000 112

  6 omega  -26.00   90.00   0.8000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3526   19.0000   30.0000 145

  7 omega  -50.00   39.60   0.8000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3526  -57.0000 -180.0000 112

  8 omega  -86.00  -11.60   0.8000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7276  142.0000   63.9235 93

  9 omega  -50.00   39.60   0.8000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3526  -57.0000    0.0000 112

 10 omega   -3.00   86.60   0.8000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3526   57.0000    0.0000 112

 11 omega  -50.00   39.60   0.8000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3526  -57.0000  -90.0000 112

 12 omega  -52.00   -8.00   0.8000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3526  -77.0000   90.0000 55

 13 omega   -3.00   86.60   0.8000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3526   57.0000  -90.0000 112

;
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0536545000
_diffrn_orient_matrix_UB_12      0.0439444000
_diffrn_orient_matrix_UB_13      -0.0188141000
_diffrn_orient_matrix_UB_21      0.0352498000
_diffrn_orient_matrix_UB_22      -0.0059160000
_diffrn_orient_matrix_UB_23      -0.0360781000
_diffrn_orient_matrix_UB_31      -0.0339673000
_diffrn_orient_matrix_UB_32      -0.0404280000
_diffrn_orient_matrix_UB_33      -0.0030215000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_sigmaI/netI    0.0705
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47211
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.02
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    25.952
_exptl_absorpt_correction_T_max  0.446
_exptl_absorpt_correction_T_min  0.084
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    4.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2553
_exptl_crystal_size_max          0.1631
_exptl_crystal_size_mid          0.0918
_exptl_crystal_size_min          0.0328
_refine_diff_density_max         5.409
_refine_diff_density_min         -2.693
_refine_diff_density_rms         0.499
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         10340
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0537P)^2^+44.7540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1428
_reflns_number_gt                7434
_reflns_number_total             10340
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02532_si_001.cif
_cod_data_source_block           K5Na2-3
_cod_original_cell_volume        2144.23(11)
_cod_database_code               4344609