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_4311153
_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            'C162 H324 K9 N18 Nb3 O54 Sb24'
_chemical_formula_weight         6941.02
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 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                 92.3650(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.0588(9)
_cell_length_b                   25.3583(8)
_cell_length_c                   38.0508(17)
_cell_measurement_reflns_used    8839
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      16.48
_cell_measurement_theta_min      2.34
_cell_volume                     25122.8(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47463
_diffrn_reflns_theta_full        15.00
_diffrn_reflns_theta_max         15.00
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82722
_exptl_absorpt_correction_type   'Empirical, SADABS'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             13488
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.708
_refine_diff_density_min         -1.227
_refine_diff_density_rms         0.219
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2146
_refine_ls_number_reflns         10110
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      2.002
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0940
_refine_ls_shift/su_max          2.292
_refine_ls_shift/su_mean         0.066
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2561
_refine_ls_wR_factor_ref         0.2918
_reflns_number_gt                7603
_reflns_number_total             10110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035397xsi20031208_113328_2.cif
_cod_data_source_block           562f1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4311153