Experimental and Theoretical Methods to Investigate Extraframework Species in a Layered Material of Dodecaniobate Anions
May Nyman; James P. Larentzos; Edward J. Maginn; Margaret E. Welk; David Ingersoll; Hyunsoo Park; John B. Parise; Ivor Bull; François Bonhomme; Inorganic Chemistry 46 (2007) 2067–2079; doi:10.1021/ic061454l

data_4306984
_publ_section_title
;
Experimental and Theoretical Methods to Investigate Extraframework Species
in a Layered Material of Dodecaniobate Anions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2067
_journal_page_last               2079
_journal_paper_doi               10.1021/ic061454l
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'Ge K10 Nb14 O50'
_chemical_formula_weight         2564.33
_space_group_IT_number           44
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      44
_symmetry_space_group_name_Hall  'I 2 -2'
_symmetry_space_group_name_H-M   'I m m 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                   10.927(2)
_cell_length_b                   11.573(2)
_cell_length_c                   19.952(4)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100K(2)
_cell_measurement_theta_max      21.88
_cell_measurement_theta_min      1.60
_cell_volume                     2523.1(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'SHELXL (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2000)'
_computing_structure_solution    'SHELXS (Sheldrick, 2000)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.871
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  'Bruker SMART 6000 CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.49595
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            2922
_diffrn_reflns_theta_full        21.88
_diffrn_reflns_theta_max         21.88
_diffrn_reflns_theta_min         1.60
_diffrn_source                   synchrotron
_diffrn_source_type              'APS beamline ID-15'
_exptl_absorpt_coefficient_mu    10.309
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.803
_refine_diff_density_min         -2.057
_refine_diff_density_rms         0.434
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(4)
_refine_ls_extinction_coef       0.00003(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2922
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          5.173
_refine_ls_shift/su_mean         0.069
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0875P)^2^+126.7785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1493
_reflns_number_gt                2922
_reflns_number_total             2922
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061454lsi20061213_043223.cif
_cod_data_source_block           new
_cod_original_cell_volume        2523.2(9)
_cod_database_code               4306984