Phosphinopnictonium Cations: High Yield and General Preparative Procedures for New Interpnictogen Frameworks Exploiting As→P and Sb→P Coordinate Bonds
Eamonn Conrad; Neil Burford; Robert McDonald; Michael J. Ferguson; Journal of the American Chemical Society 131 (2009) 17000–17008; doi:10.1021/ja907613c

data_4105376
_publ_section_title
;
 Phosphinopnictonium Cations: High Yield and General Preparative
 Procedures for New Interpnictogen Frameworks Exploiting As\\rightarrow P
 and Sb\\rightarrow P Coordinate Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17000
_journal_page_last               17008
_journal_paper_doi               10.1021/ja907613c
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C16 H19 As F3 O3 P S'
_chemical_formula_weight         454.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 96.4800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7585(8)
_cell_length_b                   12.8289(9)
_cell_length_c                   12.9423(9)
_cell_measurement_reflns_used    7932
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.21
_cell_measurement_theta_min      2.24
_cell_volume                     1939.9(2)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16071
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.982
_exptl_absorpt_correction_T_max  0.6429
_exptl_absorpt_correction_T_min  0.5468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       fragment
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4449
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0496P)^2^+0.7515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0889
_reflns_number_gt                3723
_reflns_number_total             4449
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja907613c_si_002.cif
_cod_data_source_block           dal0793
_cod_database_code               4105376