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_4330849
_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            'C147 Cu N10 O75 Si2 W20'
_chemical_formula_weight         6902.29
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.2461(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.6812(2)
_cell_length_b                   46.9386(4)
_cell_length_c                   15.7694(2)
_cell_measurement_temperature    123(2)
_cell_volume                     10619.7(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      123(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_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       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       64
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27981
_diffrn_reflns_theta_full        29.40
_diffrn_reflns_theta_max         29.40
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    10.963
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    2.159
_exptl_crystal_description       prism
_exptl_crystal_F_000             6178
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.329
_refine_diff_density_min         -2.624
_refine_diff_density_rms         0.317
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         27981
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.218
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0770
_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^)+(0.0000P)^2^+510.6225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1638
_reflns_number_gt                24912
_reflns_number_total             27981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301488a_si_002_1.cif
_cod_data_source_block           Cu-1
_cod_database_code               4330849