Structural and spectroscopic elucidation of imidazolium and pyridinium based hexachloridophosphates and niobates
Gjikaj, Mimoza; Leye, Johann-Christian; Xie, Tao; Brockner, Wolfgang; CrystEngComm 12 (2010) 1474–; doi:10.1039/b919368e

data_7212075
_publ_section_title
;
 Structural and spectroscopic elucidation of imidazolium and pyridinium
 based hexachloridophosphates and niobates
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              1474
_journal_paper_doi               10.1039/b919368e
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         '[C10NH16][PCl6]'
_chemical_formula_sum            'C10 H16 Cl6 N Nb'
_chemical_formula_weight         455.85
_chemical_name_common
;
1-butyl-4-methylpyridinium hexachloridoniobate
;
_chemical_name_systematic
;
1-butyl-4-methylpyridinium hexachloridoniobate
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.850(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1731(19)
_cell_length_b                   7.3248(7)
_cell_length_c                   16.1930(18)
_cell_measurement_reflns_used    13394
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.o2
_cell_measurement_theta_min      1.00
_cell_volume                     1761.3(3)
_computing_cell_refinement       'Stoe X-Area'
_computing_data_collection       'Stoe X-Area'
_computing_data_reduction        'Stoe X-Area'
_computing_molecular_graphics    'DIAMOND (Brandenburger, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS 2'
_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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11551
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    1.577
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.0060(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3106
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+2.4597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                2567
_reflns_number_total             3106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b919368e.txt
_cod_data_source_block           C10H16Cl6NNb
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C10 H16 Cl6 N1 Nb1'
_cod_database_code               7212075