Ternary transition-metal fluoride precursors for the fluorolytic sol-gel route: new insights into speciation and decomposition.
Kohl, J.; Wiedemann, D.; Troyanov, S. I.; Palamidis, E.; Lerch, M.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 13272–13281; doi:10.1039/c5dt01748c

data_7035535
_publ_section_title
;
 Ternary transition-metal fluoride precursors for the fluorolytic sol-gel
 route: new insights into speciation and decomposition.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13272
_journal_page_last               13281
_journal_paper_doi               10.1039/c5dt01748c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_iupac          '(C5 H6 N)[V (C5 H5 N)4 F2]Si F6'
_chemical_formula_moiety         'C20 H20 F2 N4 V 1+, F6 Si 2-, C5 H6 N 1+'
_chemical_formula_sum            'C25 H26 F8 N5 Si V'
_chemical_formula_weight         627.54
_chemical_name_systematic
'pyridinium trans-difluoridotetrakis(pyridine)vanadium(III)hexafluorosilicate'
_space_group_crystal_system      tetragonal
_space_group_IT_number           127
_space_group_name_Hall           '-P 4 2ab'
_space_group_name_H-M_alt        'P 4/m b m'
_symmetry_space_group_name_Hall  '-P 4 2ab'
_symmetry_space_group_name_H-M   'P 4/m b m'
_atom_sites_solution_hydrogens   difmap
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_audit_update_record
;
2015-06-17 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8047(2)
_cell_length_b                   10.8047(2)
_cell_length_c                   12.6865(4)
_cell_measurement_reflns_used    2992
_cell_measurement_temperature    149.9(10)
_cell_measurement_theta_max      29.1910
_cell_measurement_theta_min      4.0880
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.9(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_detector_type            'Agilent Sapphire3'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_UB_11      0.0403355000
_diffrn_orient_matrix_UB_12      -0.0107619000
_diffrn_orient_matrix_UB_13      -0.0431473000
_diffrn_orient_matrix_UB_21      0.0386566000
_diffrn_orient_matrix_UB_22      0.0490228000
_diffrn_orient_matrix_UB_23      0.0172991000
_diffrn_orient_matrix_UB_31      0.0345016000
_diffrn_orient_matrix_UB_32      -0.0422982000
_diffrn_orient_matrix_UB_33      0.0310539000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.139
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.995
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_diffrn_reflns_limit_h_max       13
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_diffrn_reflns_limit_k_min       -12
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_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2574
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.984
_diffrn_reflns_theta_min         3.772
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.449
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_exptl_absorpt_correction_T_min  0.907
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)

Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)

Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.3228
_exptl_crystal_size_mid          0.2993
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_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.844
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     60
_refine_ls_number_reflns         2574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.844
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0774P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                1293
_reflns_number_total             2574
_reflns_threshold_expression     'I > 2\s(I)'
_twin_dimensionality             triperiodic
_twin_formation_mechanism        gt
_twin_morphology                 simple
_twin_special_details
;       
Individuals are twinned by rotation of -90.5869\% around [0 0 1] in reciprocal
or (0 0 1) in direct space.
;
_cod_data_source_file            c5dt01748c1.cif
_cod_data_source_block           1c
_cod_depositor_comments
'Adding full bibliography for 7035533--7035539.cif.'
_cod_original_cell_volume        1481.04(7)
_cod_database_code               7035535
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.869
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_shelx_res_checksum              47713