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_4337692
_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
;
C21.17 H55.52 Cl6.83 Ga2 N4 P2 Si8, 4(C H2 Cl2)
;
_chemical_formula_sum            'C25.17 H63.52 Cl14.83 Ga2 N4 P2 Si8'
_chemical_formula_weight         1374.18
_chemical_name_systematic
;
 ?
;
_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                75.135(5)
_cell_angle_beta                 74.483(4)
_cell_angle_gamma                69.088(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8121(7)
_cell_length_b                   11.6925(8)
_cell_length_c                   15.0723(11)
_cell_measurement_reflns_used    7459
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      50.978
_cell_measurement_theta_min      4.531
_cell_volume                     1531.32(19)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0685
_diffrn_reflns_av_sigmaI/netI    0.0844
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43123
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         29.50
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    1.761
_exptl_absorpt_correction_T_max  0.9491
_exptl_absorpt_correction_T_min  0.4082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             699
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
The unit cell contains four heavily disordered dichloromethane molecules which 
have been treated as a diffuse contribution to the overall scattering without 
specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.737
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         8464
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0643P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                5284
_reflns_number_total             8464
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic500054w_si_002.cif
_cod_data_source_block           is_aw197
_cod_database_code               4337692