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_4344608
_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 Cs7 H58 Na2 O100 P2 W18'
_chemical_formula_weight         6418.56
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.416(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4982(5)
_cell_length_b                   12.6768(6)
_cell_length_c                   33.332(2)
_cell_measurement_reflns_used    4406
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      24.6890
_cell_measurement_theta_min      3.2120
_cell_volume                     5248.0(5)
_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 0.984
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_details
;
  1 omega  -62.00   50.00   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1683   77.0000 -120.0000 160

  2 omega   35.00   87.50   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.7933  178.0000   60.0000 75

  3 omega  -47.00  -21.80   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.7933  -57.0000   30.0000 36

  4 omega  -20.00   74.50   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.7933  -99.0000 -120.0000 135

  5 omega   42.70  112.00   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.7933  178.0000  120.0000 99

  6 omega  -98.00    3.50   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1683  -57.0000  120.0000 145

  7 omega -102.00  -25.70   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1683  -38.0000  -60.0000 109

  8 omega  -45.00   12.40   0.7000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1683  -81.0000  -52.0000 82

;
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0251869000
_diffrn_orient_matrix_UB_12      0.0479380000
_diffrn_orient_matrix_UB_13      -0.0067066000
_diffrn_orient_matrix_UB_21      0.0387348000
_diffrn_orient_matrix_UB_22      0.0069433000
_diffrn_orient_matrix_UB_23      -0.0138010000
_diffrn_orient_matrix_UB_31      -0.0336312000
_diffrn_orient_matrix_UB_32      -0.0279728000
_diffrn_orient_matrix_UB_33      -0.0149248000
_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  0.1036
_diffrn_reflns_av_sigmaI/netI    0.1009
_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       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            54167
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         29.54
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    23.249
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22077
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    4.062
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5632
_exptl_crystal_size_max          0.1010
_exptl_crystal_size_mid          0.0716
_exptl_crystal_size_min          0.0164
_platon_squeeze_details
;
Thermogravimetric analysis of the bulk sample indicated that the crystals 
contain 20 additional water molecules per unit cell (10 per formula). 
These water molecules were added in the formula of the compound and their 
diffuse contribution treated with the program SQUEEZE/PLATON.
;
_refine_diff_density_max         5.035
_refine_diff_density_min         -2.688
_refine_diff_density_rms         0.775
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.299
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         13370
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.295
_refine_ls_R_factor_all          0.1883
_refine_ls_R_factor_gt           0.1495
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3933
_refine_ls_wR_factor_ref         0.4226
_reflns_number_gt                7955
_reflns_number_total             13370
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02532_si_001.cif
_cod_data_source_block           Cs7Na2-2
_cod_database_code               4344608