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_7019796
_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            'C44 H78 Mo12 N9 O52 P Zn4'
_chemical_formula_weight         3008.88
_chemical_name_systematic
;
?
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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            2
_cell_length_a                   15.270(3)
_cell_length_b                   15.270(3)
_cell_length_c                   18.496(4)
_cell_measurement_reflns_used    8670
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.36
_cell_measurement_theta_min      1.73
_cell_volume                     4312.8(15)
_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 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0538
_diffrn_reflns_av_sigmaI/netI    0.1100
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13600
_diffrn_reflns_theta_full        30.36
_diffrn_reflns_theta_max         30.36
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    2.888
_exptl_absorpt_correction_T_max  0.6736
_exptl_absorpt_correction_T_min  0.5985
_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    2.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2430
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         1.701
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.196
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         5881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0624P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1568
_reflns_number_gt                3288
_reflns_number_total             5881
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2dt30537b.txt
_cod_data_source_block           e(bim)4
_cod_original_cell_volume        4312.6(17)
_cod_original_sg_symbol_H-M      I-4
_cod_database_code               7019796