Tetramethylphosphonium Fluoride: "Naked" Fluoride and Phosphorane
Andreas Kornath; F. Neumann; H. Oberhammer; Inorganic Chemistry 42 (2003) 2894–2901; doi:10.1021/ic020663c

data_4313536
_publ_section_title
;
 Tetramethylphosphonium Fluoride: "Naked" Fluoride and Phosphorane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2894
_journal_page_last               2901
_journal_paper_doi               10.1021/ic020663c
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C4 H20 F O4 P'
_chemical_formula_sum            'C4 H20 F O4 P'
_chemical_formula_weight         182.17
_chemical_name_systematic
;
 Tetramethylphosphoniumfluoride Tetrahydrate
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0610(10)
_cell_length_b                   11.0610(10)
_cell_length_c                   8.1630(10)
_cell_measurement_reflns_used    2332
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      30.36
_cell_measurement_theta_min      3.10
_cell_volume                     998.71(18)
_computing_cell_refinement
;
'DENZO SCALEPACK   (Otwinowski & Minor, 1997)'
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
'DENZO SCALEPACK   (Otwinowski & Minor, 1997)'
;
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material
;
SHELXL-93 (Sheldrick, 1993), Parst(Nardelli, 1983),
Platon (Spek, 1982) & Missym (Le Page, 1987)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-93 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measurement_device       'KappaCCD NONIUS'
_diffrn_measurement_method
;
330 frames via \w-rotation (\D\w=1%) and two times 150 s per frame (4 
sets at different \k-angles)
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2332
_diffrn_reflns_theta_max         30.36
_diffrn_reflns_theta_min         3.10
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.146
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.857
_refine_ls_goodness_of_fit_obs   1.045
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.857
_refine_ls_restrained_S_obs      1.045
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_obs          0.0257
_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^)+(0.0278P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0551
_refine_ls_wR_factor_obs         0.0510
_reflns_number_observed          398
_reflns_number_total             660
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020663c_2.cif
_cod_data_source_block           1661
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        998.7(2)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4313536