Cyclic oligomer of oxide clusters through a siloxane bond. Synthesis and structure of reaction products of α2-mono-lacunary Dawson polyoxometalate with tetrachlorosilane and tetraethoxysilane
Kurashina, Takayuki; Aoki, Shotaro; Hirasawa, Ryota; Hasegawa, Takeshi; Kasahara, Yuhki; Yoshida, Shoko; Yoza, Kenji; Nomiya, Kenji; Dalton Transactions  (2009) 5542–5550; doi:10.1039/b902904d

data_7001679
_publ_section_title
;
 Cyclic oligomer of oxide clusters through a siloxane bond. Synthesis
 and structure of reaction products of \a2-mono-lacunary Dawson
 polyoxometalate with tetrachlorosilane and tetraethoxysilane
;
_journal_issue                   28
_journal_name_full               'Dalton Transactions'
_journal_page_first              5542
_journal_page_last               5550
_journal_paper_doi               10.1039/b902904d
_journal_year                    2009
_chemical_formula_sum            'C26 H187 N13 O228 P6 Si6 W51'
_chemical_formula_weight         14061.60
_chemical_name_systematic
;
?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.461(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.864(10)
_cell_length_b                   37.04(2)
_cell_length_c                   21.361(13)
_cell_measurement_reflns_used    985
_cell_measurement_temperature    90
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     11760(12)
_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  0.0744
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            104845
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    25.019
_exptl_absorpt_correction_T_max  0.3677
_exptl_absorpt_correction_T_min  0.0772
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    3.971
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             12412
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         7.719
_refine_diff_density_min         -4.910
_refine_diff_density_rms         0.514
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1273
_refine_ls_number_reflns         17180
_refine_ls_number_restraints     4038
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+1332.6969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1646
_reflns_number_gt                14232
_reflns_number_total             17180
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b902904d.txt
_cod_data_source_block           tak027s-mono-p21m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        11759(13)
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               7001679