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_4330851
_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            'C144 Cu4 N14 O76 Si2 W20'
_chemical_formula_weight         7128.92
_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                 109.1160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.7374(2)
_cell_length_b                   33.6813(4)
_cell_length_c                   19.2220(3)
_cell_measurement_temperature    153(2)
_cell_volume                     11462.1(3)
_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 0.964
_diffrn_measured_fraction_theta_max 0.964
_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    0.0404
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31066
_diffrn_reflns_theta_full        29.60
_diffrn_reflns_theta_max         29.60
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    10.430
_exptl_absorpt_correction_T_max  0.3933
_exptl_absorpt_correction_T_min  0.3675
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_description       plate
_exptl_crystal_F_000             6388
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         7.433
_refine_diff_density_min         -3.858
_refine_diff_density_rms         0.290
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         31066
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0904
_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^)+(0.0600P)^2^+420.3701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2078
_refine_ls_wR_factor_ref         0.2379
_reflns_number_gt                21065
_reflns_number_total             31066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301488a_si_002_3.cif
_cod_data_source_block           Cu-4
_cod_database_code               4330851