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

data_4313535
_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_structural     'Me4 P F'
_chemical_formula_sum            'C4 H12 F P'
_chemical_formula_weight         110.11
_chemical_name_systematic        Tetramethylphosphoniumfluoride
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   10.1600(10)
_cell_length_b                   10.1800(10)
_cell_length_c                   12.0580(10)
_cell_measurement_reflns_used    7878
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.63
_cell_measurement_theta_min      3.30
_cell_volume                     1247.1(2)
_computing_cell_refinement
;
DENZO and Scalepack (Otwinowski & Minor, 1997)
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
DENZO and Scalepack (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material
;
SHELXL-93, PARST95 (Nardelli, 1995); PLATON (Spek, 2001)
;
_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       'Nonius Kappa CCD'
_diffrn_measurement_method
;
897 frames via \w-rotation (\D\w=1%) and two times 30s per frame (7 
sets at different \k-angles)
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7878
_diffrn_reflns_theta_max         25.63
_diffrn_reflns_theta_min         3.30
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.098
_refine_ls_goodness_of_fit_obs   1.153
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_restrained_S_obs      1.153
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_obs          0.0250
_refine_ls_shift/su_max          0.157
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0738
_refine_ls_wR_factor_obs         0.0722
_reflns_number_observed          1039
_reflns_number_total             1180
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020663c_1.cif
_cod_data_source_block           1080
_cod_depositor_comments
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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^)+(0.0519P)^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^)+(0.0519P)^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_database_code               4313535