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_4121089
_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            'Ge Nb13 O60 Rb13'
_chemical_formula_weight         3351.53
_chemical_name_common            'rubidium germanium tridecaniobate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   13.8490(16)
_cell_length_b                   13.8490(16)
_cell_length_c                   19.840(2)
_cell_measurement_reflns_used    493
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     3295.4(6)
_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      180(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26152
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    12.267
_exptl_absorpt_correction_T_max  0.1246
_exptl_absorpt_correction_T_min  0.0514
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker 2000'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.378
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3052
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.29
_refine_diff_density_max         3.185
_refine_diff_density_min         -2.488
_refine_diff_density_rms         0.275
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0863P)^2^+122.4496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1383
_reflns_number_gt                3793
_reflns_number_total             4526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4086484_si_004.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        3295.3(7)
_cod_database_code               4121089