Cupric Siliconiobate. Synthesis and Solid-State Studies of a Pseudosandwich-Type Heteropolyanion
Travis M. Anderson; Todd M. Alam; Mark A. Rodriguez; Joel N. Bixler; Wenqian Xu; John B. Parise; May Nyman; Inorganic Chemistry 47 (2008) 7834–7839; doi:10.1021/ic800860q

data_4305940
_publ_contact_author_email       mdnyman@sandia.gov
_publ_section_title
;
Cupric Siliconiobate. Synthesis and Solid-State Studies of a
Pseudosandwich-Type Heteropolyanion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7834
_journal_page_last               7839
_journal_paper_doi               10.1021/ic800860q
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C20 H154 Cu5 N20 Na11 Nb32 O147 Si8'
_chemical_formula_weight         6796.06
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           34
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n n 2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.992(2)
_cell_length_b                   25.426(4)
_cell_length_c                   30.046(4)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      1.65
_cell_volume                     11453(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            92463
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    2.139
_exptl_absorpt_correction_T_max  0.8145
_exptl_absorpt_correction_T_min  0.4143
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6560
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.889
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.284
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         25869
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.175
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0956P)^2^+107.8033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1768
_refine_ls_wR_factor_ref         0.1860
_reflns_number_gt                23091
_reflns_number_total             25869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800860q-file002.cif
_cod_data_source_block           siliconiobate_pseudo_sandwich
_cod_depositor_comments
;

2024-01-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C40 H308 Cu10 N40 Na22 Nb64 O294 Si16'
_cod_original_formula_weight         13592.12
_cod_original_formula_units_Z            1
_cod_database_code               4305940