Bis(<small>DL</small>-valinium) pentafluoridooxidoniobate(V)
Pushilin, M. A.; Gerasimenko, A. V.; Davidovich, R. L.; Acta Crystallographica Section E 63 (2007) m2086–m2086; doi:10.1107/S1600536807028346

data_2214580
_publ_section_title
;
 Bis(<small>DL</small>-valinium) pentafluoridooxidoniobate(V)
;
_journal_coeditor_code           CI2394
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2086
_journal_page_last               m2086
_journal_paper_doi               10.1107/S1600536807028346
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C5 H12 N O2)2 [Nb O F5]'
_chemical_formula_moiety         '2C5 H12 N O2 + , F5 Nb O 2-'
_chemical_formula_sum            'C10 H24 F5 N2 Nb O5'
_chemical_formula_weight         440.22
_chemical_name_common            'bis(DL-valinium) pentafluorooxoniobate(V)'
_chemical_name_systematic
;
(R)-1-carboxy-2-methylpropan-1-aminium (S)-1-carboxy-2-methylpropan-1-aminium
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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.1900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8018(4)
_cell_length_b                   19.4213(8)
_cell_length_c                   10.1979(4)
_cell_measurement_reflns_used    5444
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.357
_cell_measurement_theta_min      3.059
_cell_volume                     1742.01(12)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 1998)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20336
_diffrn_reflns_theta_full        31.53
_diffrn_reflns_theta_max         31.53
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.90717
_exptl_absorpt_correction_T_min  0.86121
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(SADABS and XPREP in SAINT; Bruker, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.532
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         5717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0347P)^2^+0.5786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0779
_reflns_number_gt                4829
_reflns_number_total             5717
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci2394.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2214580
_cod_database_fobs_code          2214580