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

data_7002654
_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         'C19 H54 Cl F3 N2 O3 P2 S Si8'
_chemical_formula_sum            'C19 H54 Cl F3 N2 O3 P2 S Si8'
_chemical_formula_weight         769.81
_chemical_name_common
;
1-chloro-3-triflouromethanesolfonato-2,4-
bis(tris(trimethylsilyl)silyl)-cyclo-1,3-diphospha-2,4-diazane
;
_chemical_name_systematic
;
1-chloro-3-triflouromethanesolfonato-2,4-bis[tris(trimethylsilyl)silyl]-cyclo-
1,3-diphospha-2,4-diazane
;
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.40(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.508(4)
_cell_length_b                   13.008(3)
_cell_length_c                   18.329(4)
_cell_measurement_reflns_used    8647
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      74.252
_cell_measurement_theta_min      5.471
_cell_volume                     4187.1(18)
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            70840
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.483
_exptl_absorpt_correction_T_max  0.8648
_exptl_absorpt_correction_T_min  0.7605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         12191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0638P)^2^+4.2203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1371
_reflns_number_gt                10111
_reflns_number_total             12191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b911326f.txt
_cod_data_source_block           hyp2n2p2clotf
_cod_original_cell_volume        4187.2(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7002654