Synthesis of the first fluoro(phosphanyl)- and diphosphanyl-stannanes and surprising formation of [P(SnMe3)4]+SiF5-
Driess, Matthias; Merz, Klaus; Monsé, Christian; Chemical Communications (Cambridge, United Kingdom)  (2003) 2608–2609; doi:10.1039/b308660g

data_7113634
_publ_section_title
;
 Synthesis of the first fluoro(phosphanyl)- and diphosphanyl-stannanes
 and surprising formation of [P(SnMe3)4]+SiF5-
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   20
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2608
_journal_page_last               2609
_journal_paper_doi               10.1039/b308660g
_journal_year                    2003
_chemical_formula_sum            'C60 H94 P2 Sn2'
_chemical_formula_weight         1114.67
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.08(3)
_cell_angle_beta                 91.27(3)
_cell_angle_gamma                101.45(3)
_cell_formula_units_Z            2
_cell_length_a                   10.538(4)
_cell_length_b                   16.379(7)
_cell_length_c                   17.760(7)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      16.4
_cell_measurement_theta_min      3.2
_cell_volume                     2919(2)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  'SHELXTL (Siemens, 1996)'
_computing_structure_refinement  'SHELXTL (Siemens, 1996)'
_computing_structure_solution    'SHELXTL (Siemens, 1996)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker axs CCD 1000'
_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  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24233
_diffrn_reflns_theta_full        25.66
_diffrn_reflns_theta_max         25.66
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_T_max  0.82345
_exptl_absorpt_correction_T_min  0.74532
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         10684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0414P)^2^+0.0000P] where
P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0789
_reflns_number_gt                8356
_reflns_number_total             10684
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7104854
_cod_data_source_file            b308660g.txt
_cod_data_source_block           md148
_cod_original_cell_volume        2919.4(19)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7113634