GaCl3-Assisted Cyclization Reactions in Hypersilyl(trimethylsilyl)aminodichlorophosphine
Alexander Villinger; Andrea Westenkirchner; Ronald Wustrack; Axel Schulz; Inorganic Chemistry 47 (2008) 9140–9142; doi:10.1021/ic801501c

data_4306682
_publ_contact_author_address
;
Universit\"at Rostock
Institut f\"ur Chemie
Abteilung f\"ur Anorganische Chemie
Albert-Einstein-Strasse 3a 
18059 Rostock
Bundesrepublik Deutschland
;
_publ_contact_author_email       axel.schulz@uni-rostock.de
_publ_contact_author_fax         '+49 (0)381/498-6382'
_publ_contact_author_name        'Axel Schulz'
_publ_contact_author_phone       '+49 (0)381/498-6400'
_publ_section_title
;
GaCl3-Assisted Cyclization Reactions in
Hypersilyl(trimethylsilyl)aminodichlorophosphine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9140
_journal_page_last               9142
_journal_paper_doi               10.1021/ic801501c
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C12 H36 Cl2 N P Si5'
_chemical_formula_sum            'C12 H36 Cl2 N P Si5'
_chemical_formula_weight         436.74
_chemical_name_systematic
;
N-tris-(trimethylsilyl)silyl-N-(trimethylsilyl)aminodichlorophosphane
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.45(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1800(18)
_cell_length_b                   17.440(3)
_cell_length_c                   17.069(5)
_cell_measurement_reflns_used    7828
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      70.836
_cell_measurement_theta_min      5.047
_cell_volume                     2507.0(11)
_computing_cell_refinement       'Bruker Apex v2.0-2'
_computing_data_collection       'Bruker Apex v2.0-2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
 ORTEP-3 (Farrugia, 1997), DIAMOND v3.0a (Brandenburg, 2005)
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker-Nonius Apex X8-CCD-diffractometer'
_diffrn_measurement_method       '\w 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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40850
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  0.9111
_exptl_absorpt_correction_T_min  0.6337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.053
_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     202
_refine_ls_number_reflns         9059
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0453P)^2^+0.3156P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0859
_reflns_number_gt                7223
_reflns_number_total             9059
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801501c_si_002_2.cif
_cod_data_source_block           hypntmspcl2
_cod_original_cell_volume        2507.0(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4306682