Synthesis and Reversible Transformation of Cun-Bridged (n= 1, 2, or 4) Silicodecatungstate Dimers
Kosuke Suzuki; Masahiro Shinoe; Noritaka Mizuno; Inorganic Chemistry 51 (2012) 11574–11581; doi:10.1021/ic301488a

data_4330850
_publ_contact_author_address
;
Department of Applied Chemistry, School of Engineering
The University of Tokyo
7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8656 (Japan)
;
_publ_contact_author_email       tmizuno@mail.ecc.u-tokyo.ac.jp
_publ_contact_author_fax         (+)81-3-5841-7220
_publ_contact_author_name        'Noritaka Mizuno'
_publ_contact_author_phone       (+)81-3-5841-7272
_publ_section_title
;
 Synthesis and Reversible Transformation of Cun-Bridged (n= 1, 2, or 4)
 Silicodecatungstate Dimers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11574
_journal_page_last               11581
_journal_paper_doi               10.1021/ic301488a
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C96 H0 Cu2 N6 O73 Si2 W20'
_chemical_formula_weight         6265.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 89.9710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.1007(2)
_cell_length_b                   26.6281(3)
_cell_length_c                   22.7005(3)
_cell_measurement_temperature    153(2)
_cell_volume                     10941.4(2)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            31024
_diffrn_reflns_theta_full        29.56
_diffrn_reflns_theta_max         29.56
_diffrn_reflns_theta_min         0.90
_exptl_absorpt_coefficient_mu    10.722
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_description       block
_exptl_crystal_F_000             5536
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.030
_refine_diff_density_min         -3.126
_refine_diff_density_rms         0.303
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1186
_refine_ls_number_reflns         31024
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0707
_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^)+(0.0733P)^2^+222.8782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1822
_refine_ls_wR_factor_ref         0.2077
_reflns_number_gt                23180
_reflns_number_total             31024
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301488a_si_002_2.cif
_cod_data_source_block           Cu-2
_cod_database_code               4330850