A long Nb=O double bond in bis(pyridinium) tetrachlorooxo(pyridine-κ<i>N</i>)niobate(V) chloride
Guzei, Ilia A.; Saulys, Dovas A.; Acta Crystallographica Section C 62 (2006) m369–m371; doi:10.1107/S0108270106026060

data_2015526
_publ_section_title
;
 A long Nb=O double bond in bis(pyridinium)
 tetrachlorooxo(pyridine-\k<i>N</i>)niobate(V) chloride
;
_journal_coeditor_code           SQ3030
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m369
_journal_page_last               m371
_journal_paper_doi               10.1107/S0108270106026060
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C5 H6 N)2 Cl [Nb Cl4 O (C5 H5 N)]'
_chemical_formula_moiety         'C5 H5 Cl4 N Nb O - , 2C5 H6 N + , Cl -'
_chemical_formula_sum            'C15 H17 Cl5 N3 Nb O'
_chemical_formula_weight         525.48
_chemical_name_systematic
;
bis(pyridinium) (tetrachloro-oxo-pyridine-\kN)niobate(V) chloride
;
_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                 99.328(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6122(9)
_cell_length_b                   20.091(2)
_cell_length_c                   13.8061(16)
_cell_measurement_reflns_used    12954
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.3680
_cell_measurement_theta_min      2.5191
_cell_volume                     2083.5(4)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area-detector'
_diffrn_measurement_method       '0.30\% \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16884
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.228
_exptl_absorpt_correction_T_max  0.66
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.33
_refine_diff_density_max         1.436
_refine_diff_density_min         -0.962
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0377P)^2^+2.8236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0792
_reflns_number_gt                4097
_reflns_number_total             4257
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sq3030.cif
_cod_data_source_block           II
_cod_database_code               2015526
_cod_database_fobs_code          2015526