Heterometallic 3d-4f cubane clusters inserted in polyoxometalate matrices.
Nohra, Brigitte; Mialane, Pierre; Dolbecq, Anne; Rivière, Eric; Marrot, Jérôme; Sécheresse, Francis; Chemical communications (Cambridge, England) 34 (2009) 2703–2705; doi:10.1039/b902094b

data_7104426
_publ_section_title
;
 Heterometallic 3d-4f cubane clusters inserted in polyoxometalate
 matrices.
;
_journal_issue                   19
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2703
_journal_page_last               2705
_journal_paper_doi               10.1039/b902094b
_journal_volume                  34
_journal_year                    2009
_chemical_formula_sum            'C20 H130 Cu8 La2 N20 O106 Si2 W22'
_chemical_formula_weight         7234.17
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.1940(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.2396(6)
_cell_length_b                   19.0111(10)
_cell_length_c                   23.3826(12)
_cell_measurement_reflns_used    17620
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      1.38
_cell_volume                     5418.5(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCDC area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_sigmaI/netI    0.1097
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            41717
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    25.691
_exptl_absorpt_correction_T_max  0.1832
_exptl_absorpt_correction_T_min  0.0793
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    4.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             6372
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.591
_refine_diff_density_min         -3.371
_refine_diff_density_rms         0.492
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         15683
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0318P)^2^+24.5029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                9769
_reflns_number_total             15683
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b902094b.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7104426