Preparation and Properties of Dimethyltetrafluorophosphate
Christian Hohenstein; Andreas Kornath; Frank Neumann; Ralf Ludwig; Inorganic Chemistry 49 (2010) 6421–6427; doi:10.1021/ic902438e

data_4316102
_publ_contact_author_address
;Department of Chemistry and Biochemistry, 
Ludwig-Maximilians-University, 
Butenandtstrasse 5-13, 
81377 Munich, Germany
;
_publ_contact_author_email       andreas.kornath@cup.uni-muenchen.de
_publ_contact_author_fax         +4989218077487
_publ_contact_author_name        'Andreas Kornath'
_publ_contact_author_phone       +4989218077481
_publ_section_title
;
 Preparation and Properties of Dimethyltetrafluorophosphate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6421
_journal_page_last               6427
_journal_paper_doi               10.1021/ic902438e
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         C4H12N+C2H6F4P
_chemical_formula_sum            'C6 H18 F4 N P'
_chemical_formula_weight         211.18
_chemical_name_systematic
'tetramethylammonium hdimethyltetrafluorophosphate'
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.035(3)
_cell_length_b                   7.998(2)
_cell_length_c                   10.238(2)
_cell_measurement_temperature    157(2)
_cell_volume                     1067.4(4)
_computing_cell_refinement       'SCALEPACK (Minor, Otwinowski)'
_computing_data_collection       'SCALEPACK (Minor, Otwinowski)'
_computing_molecular_graphics    'SHELXS-86 (Sheldrick, 1990)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      157(2)
_diffrn_measurement_device       'Enraf Nonius Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            1989
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.53
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.268
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       '0.05 x 0.06 x 0.1 mm'
_exptl_crystal_F_000             448
_exptl_crystal_recrystallization_method acetonitrile
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.945
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1064
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.379
_refine_ls_restrained_S_obs      1.088
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_obs          0.0325
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2132
_refine_ls_wR_factor_obs         0.0797
_reflns_number_observed          787
_reflns_number_total             1126
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic902438e_si_001.cif
_cod_data_source_block           1891b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0479P)^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^)+(0.0479P)^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               4316102