Synthesis and Structure of Dawson Polyoxometalate-Based, Multifunctional, Inorganic-Organic Hybrid Compounds: Organogermyl Complexes with One Terminal Functional Group and Organosilyl Analogues with Two Terminal Functional Groups
Kenji Nomiya; Yoshihiro Togashi; Yuhki Kasahara; Shotaro Aoki; Hideaki Seki; Marie Noguchi; Shoko Yoshida; Inorganic Chemistry 50 (2011) 9606–9619; doi:10.1021/ic201336v

data_4326383
_publ_section_title
;
 Synthesis and Structure of Dawson Polyoxometalate-Based, Multifunctional,
 Inorganic-Organic Hybrid Compounds: Organogermyl Complexes with One
 Terminal Functional Group and Organosilyl Analogues with Two Terminal
 Functional Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9606
_journal_page_last               9619
_journal_paper_doi               10.1021/ic201336v
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C36 H140 N12 O136 P4 Si4 W34'
_chemical_formula_weight         9304.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.08(3)
_cell_angle_beta                 88.92(3)
_cell_angle_gamma                76.63(3)
_cell_formula_units_Z            2
_cell_length_a                   13.284(3)
_cell_length_b                   25.075(5)
_cell_length_c                   26.170(5)
_cell_measurement_reflns_used    990
_cell_measurement_temperature    90
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      2.23
_cell_volume                     7846(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            70133
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         0.84
_exptl_absorpt_coefficient_mu    24.990
_exptl_absorpt_correction_T_max  0.6348
_exptl_absorpt_correction_T_min  0.0498
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.966
_exptl_crystal_description       needle-crystals
_exptl_crystal_F_000             8280
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.994
_refine_diff_density_min         -1.924
_refine_diff_density_rms         0.365
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1869
_refine_ls_number_reflns         22567
_refine_ls_number_restraints     5574
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+276.7560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1049
_reflns_number_gt                19234
_reflns_number_total             22567
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201336v_si_002_4.cif
_cod_data_source_block           yto001bs-tri
_cod_database_code               4326383