Hypersilylated cyclodiphosphadiazanes and cyclodiphosphadiazenium salts
Kuzora, René; Schulz, Axel; Villinger, Alexander; Wustrack, Ronald; Dalton Transactions  (2009) 9304–; doi:10.1039/b911326f

data_7002653
_publ_section_title
;
 Hypersilylated cyclodiphosphadiazanes and cyclodiphosphadiazenium
 salts
;
_journal_issue                   42
_journal_name_full               'Dalton Transactions'
_journal_page_first              9304
_journal_paper_doi               10.1039/b911326f
_journal_year                    2009
_chemical_formula_moiety         'C9 H28 Cl2 N P Si4'
_chemical_formula_sum            'C9 H28 Cl2 N P Si4'
_chemical_formula_weight         364.55
_chemical_name_common
N-(tris(trimethylsilyl)silyl)amino(dichloro)phosphane
_chemical_name_systematic
;
N-[tris(trimethylsilyl)silyl]amino(dichloro)phosphane
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.80(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.513(3)
_cell_length_b                   9.906(2)
_cell_length_c                   27.600(6)
_cell_measurement_reflns_used    9786
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      57.300
_cell_measurement_theta_min      4.864
_cell_volume                     4240.9(15)
_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)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            27606
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.9376
_exptl_absorpt_correction_T_min  0.7025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         6166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0540P)^2^+1.8812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                4528
_reflns_number_total             6166
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b911326f.txt
_cod_data_source_block           hypnhpcl2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7002653