Observing Assembly of Complex Inorganic Materials from Polyoxometalate Building Blocks
Yu Hou; Lev N. Zakharov; May Nyman; Journal of the American Chemical Society 135 (2013) 16651–16657; doi:10.1021/ja4086484

data_4121087
_publ_contact_author_address
;Oregon State University
Department of Chemistry
153 Gilbert Hall
Corvallis, OR, USA 97331
;
_publ_contact_author_email       May.Nyman@oregonstate.edu
_publ_contact_author_name        'Dr. May NYMAN'
_publ_section_title
;
 Observing Assembly of Complex Inorganic Materials from Polyoxometalate
 Building Blocks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16651
_journal_page_last               16657
_journal_paper_doi               10.1021/ja4086484
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'Cs18 Nb26 O120 Si2'
_chemical_formula_weight         6784.22
_chemical_name_common            'cesium silicon tridecaniobate dimer'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                115.596(4)
_cell_angle_beta                 95.958(3)
_cell_angle_gamma                101.551(4)
_cell_formula_units_Z            1
_cell_length_a                   13.043(3)
_cell_length_b                   19.407(8)
_cell_length_c                   19.475(5)
_cell_measurement_reflns_used    382
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     4254(2)
_computing_cell_refinement       'SMART 5.054 (Bruker, 1998)'
_computing_data_collection       'SMART 5.054 (Bruker, 1998)'
_computing_data_reduction        'SAINT 6.02 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL 5.1  (Bruker, 1998)'
_computing_publication_material  'SHELXTL 5.1  (Bruker, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL 5.1  (Bruker, 1998'
_diffrn_ambient_temperature      188(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1486
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18026
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    5.575
_exptl_absorpt_correction_T_max  0.5243
_exptl_absorpt_correction_T_min  0.2227
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker 2000'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.649
_exptl_crystal_description       oval
_exptl_crystal_F_000             3044
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_refine_diff_density_max         4.625
_refine_diff_density_min         -4.219
_refine_diff_density_rms         0.654
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.513
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         18026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.513
_refine_ls_R_factor_all          0.2561
_refine_ls_R_factor_gt           0.1761
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4531
_refine_ls_wR_factor_ref         0.4955
_reflns_number_gt                9392
_reflns_number_total             18026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4086484_si_002.cif
_cod_data_source_block           11jn042
_cod_original_cell_volume        4253(2)
_cod_database_code               4121087