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_4326382
_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            'C18 H66 N6 O70 P2 Si2 W17'
_chemical_formula_weight         4730.34
_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                 107.7830(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.0572(15)
_cell_length_b                   13.4340(8)
_cell_length_c                   26.7558(17)
_cell_measurement_reflns_used    9217
_cell_measurement_temperature    90
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.20
_cell_volume                     8233.9(9)
_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      90
_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  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            86342
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    23.818
_exptl_absorpt_correction_T_max  0.3822
_exptl_absorpt_correction_T_min  0.0629
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    3.816
_exptl_crystal_density_meas      0
_exptl_crystal_description       rod
_exptl_crystal_F_000             8368
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         13.101
_refine_diff_density_min         -2.109
_refine_diff_density_rms         0.471
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     976
_refine_ls_number_reflns         20497
_refine_ls_number_restraints     1350
_refine_ls_restrained_S_all      3.934
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          2.825
_refine_ls_shift/su_mean         0.027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+297.4701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                17933
_reflns_number_total             20497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201336v_si_002_3.cif
_cod_data_source_block           mn002mono
_cod_database_code               4326382