Disordering of the [NbOF~5~]^2{-^} complex anions in bis(glycinium) pentafluoridooxidoniobate(V) and bis(β-alaninium) pentafluoridooxidoniobate(V) dihydrate
Gerasimenko, A. V.; Pushilin, M. A.; Davidovich, R. L.; Acta Crystallographica Section C 64 (2008) m358–m361; doi:10.1107/S0108270108026413

data_2016840
_publ_section_title
;
 Disordering of the [NbOF~5~]^2{-^} complex anions in bis(glycinium)
 pentafluoridooxidoniobate(V) and bis(\b-alaninium)
 pentafluoridooxidoniobate(V) dihydrate
;
_journal_coeditor_code           SF3082
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m358
_journal_page_last               m361
_journal_paper_doi               10.1107/S0108270108026413
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '(C2 H6 N O2)2 [Nb O F5]'
_chemical_formula_moiety         '2(C2 H6 N O2 +), F5 Nb O 2-'
_chemical_formula_sum            'C4 H12 F5 N2 Nb O5'
_chemical_formula_weight         356.07
_chemical_name_common            'bis(glycinium) pentafluoridooxidoniobate(V)'
_chemical_name_systematic
;
bis(glycinium) pentafluoridooxidoniobate(V)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.0220(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.35320(10)
_cell_length_b                   10.8585(3)
_cell_length_c                   8.9913(2)
_cell_measurement_reflns_used    1882
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      50.495
_cell_measurement_theta_min      3.753
_cell_volume                     522.64(2)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19292
_diffrn_reflns_theta_full        45.00
_diffrn_reflns_theta_max         50.50
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    1.241
_exptl_absorpt_correction_T_max  0.7227
_exptl_absorpt_correction_T_min  0.6689
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       spherical
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.28
_exptl_crystal_size_rad          0.14
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.951
_refine_ls_extinction_coef       0.0379(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         5525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.0886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0748
_reflns_number_gt                5027
_reflns_number_total             5525
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sf3082.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               2016840
_cod_database_fobs_code          2016840