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_7104424
_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 Gd2 N20 O106 Si2 W22'
_chemical_formula_weight         7270.87
_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                 92.876(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.8772(12)
_cell_length_b                   24.024(2)
_cell_length_c                   18.6102(17)
_cell_measurement_reflns_used    25437
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.31
_cell_measurement_theta_min      1.39
_cell_volume                     6196.7(10)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            48111
_diffrn_reflns_theta_full        30.31
_diffrn_reflns_theta_max         30.31
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    22.846
_exptl_absorpt_correction_T_max  0.2084
_exptl_absorpt_correction_T_min  0.2084
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.849
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             6408
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.430
_refine_diff_density_min         -2.851
_refine_diff_density_rms         0.375
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         18200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+16.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                12661
_reflns_number_total             18200
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b902094b.txt
_cod_data_source_block           1a
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7104424