An Approach to the Synthesis of Polyoxometalate Encapsulating Different Kinds of Oxoanions as Heteroions: Bisphosphitopyrophosphatotriacontamolybdate [(HPO3)2(P2O7)Mo30O90]8-
Sayuri Maeda; Takuya Goto; Masayo Takamoto; Kazuo Eda; Sadayuki Himeno; Hiroki Takahashi; Toshitaka Hori; Inorganic Chemistry 47 (2008) 11197–11201; doi:10.1021/ic801499y

data_4306680
_publ_section_title
;
An Approach to the Synthesis of Polyoxometalate Encapsulating Different
Kinds of Oxoanions as Heteroions:
Bisphosphitopyrophosphatotriacontamolybdate [(HPO3)2(P2O7)Mo30O90]8-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11197
_journal_page_last               11201
_journal_paper_doi               10.1021/ic801499y
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C96 H226 Mo30 N8 O103 P4'
_chemical_formula_weight         6142.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   30.827(2)
_cell_length_b                   22.8060(15)
_cell_length_c                   30.928(2)
_cell_measurement_reflns_used    22152
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.727
_cell_measurement_theta_min      3.185
_cell_volume                     21744(2)
_computing_cell_refinement       'Bruker AXS SAINT'
_computing_data_collection       'Bruker AXS SAINT'
_computing_data_reduction        'Bruker AXS SAINT'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_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  0.0847
_diffrn_reflns_av_sigmaI/netI    0.0821
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            101747
_diffrn_reflns_theta_full        26.89
_diffrn_reflns_theta_max         26.89
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    1.773
_exptl_absorpt_correction_T_max  0.7525
_exptl_absorpt_correction_T_min  0.6183
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'program SADABS ver. 2.03(Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             12008
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         5.194
_refine_diff_density_min         -3.438
_refine_diff_density_rms         0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1085
_refine_ls_number_reflns         22331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.2111
_refine_ls_R_factor_gt           0.1147
_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^)+(0.0000P)^2^+1581.7136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2305
_refine_ls_wR_factor_ref         0.2921
_reflns_number_gt                12094
_reflns_number_total             22331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801499y_si_001.cif
_cod_data_source_block           16goc
_cod_original_cell_volume        21743(3)
_cod_database_code               4306680