Coordination complexes of the dimethyl-thio-phosphonium cation and ligand exchange.
Weigand, Jan J.; Burford, Neil; Mahnke, Devin; Decken, Andreas; Inorganic chemistry 46 (2007) 7689–7691; doi:10.1021/ic7012792

data_4339763
_publ_section_title
;
 Coordination complexes of the dimethyl-thio-phosphonium cation and ligand
 exchange.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7689
_journal_page_last               7691
_journal_paper_doi               10.1021/ic7012792
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C10 H16 F3 N2 O3 P S2'
_chemical_formula_weight         364.34
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                98.446(5)
_cell_angle_beta                 97.670(5)
_cell_angle_gamma                91.537(5)
_cell_formula_units_Z            4
_cell_length_a                   9.297(3)
_cell_length_b                   11.347(4)
_cell_length_c                   15.335(5)
_cell_measurement_reflns_used    5219
_cell_measurement_temperature    198(1)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.43
_cell_volume                     1584.1(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      198(1)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6924
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.36
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Kristalloflex 760'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  0.9765
_exptl_absorpt_correction_T_min  0.8507
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997b)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                4678
_reflns_number_total             6924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7012792.cif
_cod_data_source_block           nb060876
_cod_original_cell_volume        1584.0(9)
_cod_database_code               4339763