Synthesis of 1,3-Dichloro-cyclo-1,3-diphosphadiazanes from Silylated Amino(dichloro)phosphanes
Axel Schulz; Alexander Villinger; Andrea Westenkirchner; Inorganic Chemistry 52 (2013) 11457–11468; doi:10.1021/ic4017728

data_4336285
_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'
_publ_section_title
;
 Synthesis of 1,3-Dichloro-cyclo-1,3-diphosphadiazanes from Silylated
 Amino(dichloro)phosphanes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11457
_journal_page_last               11468
_journal_paper_doi               10.1021/ic4017728
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C22 H25 N Si'
_chemical_formula_sum            'C22 H25 N Si'
_chemical_formula_weight         331.52
_chemical_name_systematic
;
Triphenylmethylamino-trimethylsilane
;
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_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Villinger, A.'
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_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      60.739
_cell_measurement_theta_min      4.948
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_computing_cell_refinement       'Bruker Apex V7.51A'
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_computing_publication_material  SHELXL-97
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_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 Apex Kappa II-CCD-diffractometer'
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_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_max       14
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_diffrn_reflns_limit_l_min       -15
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_diffrn_reflns_theta_max         30.00
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_exptl_absorpt_correction_T_max  0.9900
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
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_exptl_crystal_description       needle
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.312
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_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         5572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0550P)^2^+0.1367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                4362
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_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic4017728_si_001_05.cif
_cod_data_source_block           av_aw111b_tritylNHSiMe3
_cod_original_cell_volume        954.96(9)
_cod_database_code               4336285