Gas Phase, Solution, and Solid State Alkali Ion Binding by the [NbE8]3- (E = As, Sb) Complexes: Synthesis, Structure, and Spectroscopy
Banu Kesanli; James Fettinger; Brian Scott; Bryan Eichhorn; Inorganic Chemistry 43 (2004) 3840–3846; doi:10.1021/ic035397x

data_4311152
_publ_section_title
;
 Gas Phase, Solution, and Solid State Alkali Ion Binding by the [NbE8]3-
 (E = As, Sb) Complexes: Synthesis, Structure, and Spectroscopy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3840
_journal_page_last               3846
_journal_paper_doi               10.1021/ic035397x
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C56 H116 As8 K3 N8 Nb O18'
_chemical_formula_weight         1999.14
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.01
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.243(4)
_cell_length_b                   23.090(4)
_cell_length_c                   19.265(4)
_cell_measurement_temperature    193(2)
_cell_volume                     8114(3)
_computing_cell_refinement       'XSCANS 2.10 b (Siemens)'
_computing_data_collection       'XSCANS 2.10 b (Siemens)'
_computing_data_reduction        'XSCANS 2.10 b (Siemens)'
_computing_molecular_graphics    'SHELXTL PC 4.2/360 (Siemens)'
_computing_publication_material  'SHELXTL PC 4.2/360 (Siemens)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0567
_diffrn_reflns_av_sigmaI/netI    0.1084
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            13549
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        '< 2'
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.604
_exptl_absorpt_correction_T_max  0.4429
_exptl_absorpt_correction_T_min  0.2939
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4056
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         10482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+4.8089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                6310
_reflns_number_total             10482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035397xsi20031208_113328_1.cif
_cod_data_source_block           NbAs8
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4311152