The Reactivity of Silylated Amino(dichloro)phosphanes in the Presence of Silver Salts.
Schulz, Axel; Villinger, Alexander; Westenkirchner, Andrea; Inorganic chemistry 53 (2014) 3183–3193; doi:10.1021/ic500054w

data_4337691
_publ_section_title
;
 The Reactivity of Silylated Amino(dichloro)phosphanes in the Presence of
 Silver Salts.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3183
_journal_page_last               3193
_journal_paper_doi               10.1021/ic500054w
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C60 H108 Ag4 Cl4 F20 N4 P4 Si16'
_chemical_formula_sum            'C60 H108 Ag4 Cl4 F20 N4 P4 Si16'
_chemical_formula_weight         2412.10
_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                73.7960(10)
_cell_angle_beta                 88.5870(10)
_cell_angle_gamma                89.9520(10)
_cell_formula_units_Z            2
_cell_length_a                   14.7631(2)
_cell_length_b                   14.7767(2)
_cell_length_c                   24.6511(4)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      56.569
_cell_measurement_theta_min      5.515
_cell_volume                     5162.33(13)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0847
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            173195
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         0.86
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_T_max  0.9122
_exptl_absorpt_correction_T_min  0.8440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         37217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+2.6029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                22342
_reflns_number_total             37217
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic500054w_si_002.cif
_cod_data_source_block           av_aw208c
_cod_database_code               4337691