The Tris(trifluoromethyl)methyl Phosphonium Ion, P(CF3)3CH3+, Preparation and Structure
Oleg Shyshkov; Uwe Dieckbreder; Thomas Drews; Alexander Kolomeitsev; Gerd-Volker Röschenthaler; Konrad Seppelt; Inorganic Chemistry 48 (2009) 6083–6085; doi:10.1021/ic900414q

data_4302502
_publ_section_title
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The Tris(trifluoromethyl)methyl Phosphonium Ion, P(CF3)3CH3+, Preparation
and Structure
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6083
_journal_page_last               6085
_journal_paper_doi               10.1021/ic900414q
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C4 H3 F9 P, F11 Sb2'
_chemical_formula_sum            'C4 H3 F20 P Sb2'
_chemical_formula_weight         705.53
_chemical_name_systematic
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 Methyl-tris(trifluoromethyl)phosphonium undecafluorodiantimonate
;
_chemical_temperature_decomposition 383.15
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.5219(19)
_cell_length_b                   13.664(2)
_cell_length_c                   17.597(3)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.0
_cell_volume                     3251.3(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Bruker_CCD
_diffrn_measurement_method       omega_scan
_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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            51535
_diffrn_reflns_theta_full        30.54
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.624
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker_2000_NT_Software_Reference_Manual
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.883
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          .1
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .03
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       0.000058(17)
_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   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0187P)^2^+13.1093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                3345
_reflns_number_total             4976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900414q_si_001.cif
_cod_data_source_block           pch3cf3
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been given
as '110C_decomp'. The value '110C_decomp' was changed to '383.15' -
it was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_database_code               4302502