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_4326380
_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            'C17 H63 Ge N7 O64 P2 W17'
_chemical_formula_weight         4649.72
_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                75.146(6)
_cell_angle_beta                 88.619(6)
_cell_angle_gamma                68.397(6)
_cell_formula_units_Z            2
_cell_length_a                   13.346(5)
_cell_length_b                   13.361(5)
_cell_length_c                   25.664(10)
_cell_measurement_reflns_used    8822
_cell_measurement_temperature    90
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.24
_cell_volume                     4100(3)
_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 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            69450
_diffrn_reflns_theta_full        28.53
_diffrn_reflns_theta_max         28.53
_diffrn_reflns_theta_min         0.82
_exptl_absorpt_coefficient_mu    24.235
_exptl_absorpt_correction_T_max  0.3771
_exptl_absorpt_correction_T_min  0.1590
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.766
_exptl_crystal_density_meas      0
_exptl_crystal_description       plate-crystals
_exptl_crystal_F_000             4092
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         8.429
_refine_diff_density_min         -2.759
_refine_diff_density_rms         0.640
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     957
_refine_ls_number_reflns         20216
_refine_ls_number_restraints     2826
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0966P)^2^+109.2124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1634
_reflns_number_gt                16018
_reflns_number_total             20216
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201336v_si_002_1.cif
_cod_data_source_block           yka015s
_cod_database_code               4326380