ε-Keggin-based coordination networks: Synthesis, structure and application toward green synthesis of polyoxometalate@graphene hybrids.
Rodriguez-Albelo, L Marleny; Rousseau, Guillaume; Mialane, Pierre; Marrot, Jérôme; Mellot-Draznieks, Caroline; Ruiz-Salvador, A Rabdel; Li, Shiwen; Liu, Rongji; Zhang, Guangjin; Keita, Bineta; Dolbecq, Anne; Dalton transactions (Cambridge, England : 2003) 41 (2012) 9989–9999; doi:10.1039/c2dt30537b

data_7019794
_publ_section_title
;
 \e-Keggin-based coordination networks: Synthesis, structure and
 application toward green synthesis of polyoxometalate@graphene hybrids.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9989
_journal_page_last               9999
_journal_paper_doi               10.1039/c2dt30537b
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C64 H120 Mo12 N3 O48.5 P Zn4'
_chemical_formula_weight         3151.36
_chemical_name_systematic
;
?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.899(5)
_cell_length_b                   20.306(5)
_cell_length_c                   22.900(5)
_cell_measurement_reflns_used    35339
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.87
_cell_measurement_theta_min      1.37
_cell_volume                     10183(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 512x512
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD 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  0.0654
_diffrn_reflns_av_sigmaI/netI    0.3137
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            62280
_diffrn_reflns_theta_full        29.87
_diffrn_reflns_theta_max         29.87
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    2.447
_exptl_absorpt_correction_T_max  0.7926
_exptl_absorpt_correction_T_min  0.6413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G. M. Sheldrick, SADABS; program for scaling and correction of area detector data, University of G ttingen, Germany, 1997'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             5556
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         3.089
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.161
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.024(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         26789
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1771
_refine_ls_wR_factor_ref         0.2293
_reflns_number_gt                19926
_reflns_number_total             26789
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2dt30537b.txt
_cod_data_source_block           e(isop)2
_cod_original_sg_symbol_H-M      Pna21
_cod_original_formula_sum        'C64 H120 Mo12 N3 O48.50 P Zn4'
_cod_database_code               7019794