Lewis Acid Assisted Methyl/Chlorine Exchange in Silylated Hydrazinochlorophosphanes
Andrea Westenkirchner; Alexander Villinger; Konstantin Karaghiosoff; Ronald Wustrack; Dirk Michalik; Axel Schulz; Inorganic Chemistry 50 (2011) 2691–2702; doi:10.1021/ic200005q

data_4324729
_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, alexander.villinger@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 or 6403'
_publ_section_title
;
 Lewis Acid Assisted Methyl/Chlorine Exchange in Silylated
 Hydrazinochlorophosphanes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2691
_journal_page_last               2702
_journal_paper_doi               10.1021/ic200005q
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C16 H35 Cl3 Ga N2 P Si3'
_chemical_formula_sum            'C16 H35 Cl3 Ga N2 P Si3'
_chemical_formula_weight         546.77
_chemical_name_systematic
;
N,N',N'-tris(trimethylsilyl)hydrazino-methyl(phenyl)phosphane 
galliumtrichloride addukt
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.759(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8091(3)
_cell_length_b                   15.7487(5)
_cell_length_c                   17.4956(6)
_cell_measurement_reflns_used    9050
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      64.782
_cell_measurement_theta_min      4.944
_cell_volume                     2663.62(15)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            47351
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    1.535
_exptl_absorpt_correction_T_max  0.6821
_exptl_absorpt_correction_T_min  0.5583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.132
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         9630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0431P)^2^+0.6060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0820
_reflns_number_gt                7860
_reflns_number_total             9630
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic200005q_si_001_6.cif
_cod_data_source_block           nnpmeph_gacl3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4324729