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_4344610
_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            'Co7 H94 Na15 O162 P4 W30'
_chemical_formula_weight         9083.49
_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                101.199(2)
_cell_angle_beta                 93.011(2)
_cell_angle_gamma                105.768(2)
_cell_formula_units_Z            1
_cell_length_a                   12.7112(3)
_cell_length_b                   12.7409(4)
_cell_length_c                   23.7998(6)
_cell_measurement_reflns_used    17801
_cell_measurement_temperature    120.00(14)
_cell_measurement_theta_max      30.0240
_cell_measurement_theta_min      2.9113
_cell_volume                     3616.05(18)
_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(14)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_details
;
  1 omega    9.00   36.00   0.6000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9465   57.0000 -150.0000 45

  2 omega  -38.00   17.20   0.6000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9465   57.0000   90.0000 92

  3 omega   28.00   61.60   0.6000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7277  -99.0000  120.0000 56

  4 omega   34.00   62.20   0.6000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7277  -99.0000 -120.0000 47

  5 omega   -5.00   87.40   0.6000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7277   38.0000  -60.0000 154

  6 omega    6.00   33.00   0.6000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7277  -99.0000    0.0000 45

  7 omega   -8.00   88.00   0.6000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7277   77.0000    0.0000 160

  8 omega  -52.00   45.20   0.6000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7277  -38.0000  120.0000 162

  9 omega  -40.00   47.60   0.6000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9465   57.0000  -90.0000 146

 10 omega  -96.00  -36.00   0.6000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9465 -178.0000 -120.0000 100

 11 omega   35.00   95.60   0.6000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7277  178.0000 -120.0000 101

 12 omega   -9.00   90.00   0.6000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7277   77.0000 -120.0000 165

 13 omega   -9.00   90.00   0.6000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7277   77.0000   30.0000 165

 14 omega   -5.00   91.60   0.6000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7277   38.0000 -180.0000 161

 15 omega  -49.00   46.40   0.6000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7277  -77.0000  150.0000 159

 16 omega  -20.00   61.60   0.6000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7277  -99.0000   30.0000 136

;
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0364085000
_diffrn_orient_matrix_UB_12      -0.0111456000
_diffrn_orient_matrix_UB_13      -0.0204214000
_diffrn_orient_matrix_UB_21      -0.0011559000
_diffrn_orient_matrix_UB_22      0.0486351000
_diffrn_orient_matrix_UB_23      -0.0100241000
_diffrn_orient_matrix_UB_31      0.0455796000
_diffrn_orient_matrix_UB_32      0.0319693000
_diffrn_orient_matrix_UB_33      0.0204239000
_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  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            89739
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    24.745
_exptl_absorpt_correction_T_max  0.671
_exptl_absorpt_correction_T_min  0.062
_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            orange
_exptl_crystal_density_diffrn    4.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4024
_exptl_crystal_size_max          0.1936
_exptl_crystal_size_mid          0.1279
_exptl_crystal_size_min          0.0164
_platon_squeeze_details
;
According to TGA, 6 additional water molecules were added to the unit cell 
which were treated as a diffuse contribution to the overall scattering without 
specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         8.361
_refine_diff_density_min         -2.851
_refine_diff_density_rms         0.446
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     985
_refine_ls_number_reflns         19371
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+189.1526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1136
_reflns_number_gt                14868
_reflns_number_total             19371
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02532_si_001.cif
_cod_data_source_block           Na15-4
_cod_original_cell_volume        3616.04(17)
_cod_database_code               4344610