#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:37:30 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179730 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/26/7002656.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7002656
loop_
_publ_author_name
'Kuzora, René'
'Schulz, Axel'
'Villinger, Alexander'
'Wustrack, Ronald'
_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 H27 Cl Si4'
_chemical_formula_sum            'C9 H27 Cl Si4'
_chemical_formula_weight         283.12
_chemical_name_common            Tris(trimethylsilyl)silylchloride
_chemical_name_systematic
;
Tris(trimethylsilyl)silylchloride
;
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      205
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.467(3)
_cell_length_b                   15.467(3)
_cell_length_c                   15.467(3)
_cell_measurement_reflns_used    1856
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      58.002
_cell_measurement_theta_min      8.732
_cell_volume                     3700.1(12)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa Apex 2-CCD-diffractometer'
_diffrn_measurement_method       'ω 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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7244
_diffrn_reflns_theta_full        28.99
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         4.93
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  0.8755
_exptl_absorpt_correction_T_min  0.8400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.148
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         1628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0349
_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/[σ²(Fo²)+(0.0525P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                1198
_reflns_number_total             1628
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            b911326f.txt
_cod_data_source_block           hypcl
_cod_original_cell_volume        3700.3(12)
_cod_original_sg_symbol_H-M      'P a-3'
_cod_database_code               7002656
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.15807(2) 0.15807(2) 0.15807(2) 0.02720(16) Uani 1 3 d S . .
Cl Cl 0.23739(2) 0.23739(2) 0.23739(2) 0.03709(17) Uani 1 3 d S . .
Si2 Si 0.19486(3) 0.19361(3) 0.01566(3) 0.04463(17) Uani 1 1 d . . .
C2 C 0.13038(13) 0.12538(14) -0.06013(11) 0.0687(6) Uani 1 1 d . . .
H2A H 0.0686 0.1354 -0.0502 0.103 Uiso 1 1 calc R . .
H2B H 0.1437 0.0643 -0.0501 0.103 Uiso 1 1 calc R . .
H2C H 0.1449 0.1406 -0.1199 0.103 Uiso 1 1 calc R . .
C1 C 0.1731(2) 0.30993(13) -0.00578(14) 0.1025(11) Uani 1 1 d . . .
H1A H 0.1945 0.3251 -0.0634 0.154 Uiso 1 1 calc R . .
H1B H 0.2026 0.3453 0.0377 0.154 Uiso 1 1 calc R . .
H1C H 0.1107 0.3206 -0.0029 0.154 Uiso 1 1 calc R . .
C3 C 0.31258(15) 0.1762(2) -0.00277(13) 0.0986(10) Uani 1 1 d . . .
H3A H 0.3260 0.1146 0.0030 0.148 Uiso 1 1 calc R . .
H3B H 0.3457 0.2092 0.0400 0.148 Uiso 1 1 calc R . .
H3C H 0.3280 0.1958 -0.0610 0.148 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Si1 0.02720(16) 0.02720(16) 0.02720(16) -0.00125(13) -0.00125(13) -0.00125(13)
Cl 0.03709(17) 0.03709(17) 0.03709(17) -0.00603(13) -0.00603(13) -0.00603(13)
Si2 0.0563(3) 0.0514(3) 0.0262(2) -0.00217(18) -0.00076(18) -0.0129(2)
C2 0.0840(14) 0.0853(14) 0.0367(8) -0.0121(9) -0.0073(9) -0.0243(12)
C1 0.204(3) 0.0580(13) 0.0458(11) 0.0151(10) -0.0092(14) -0.0120(16)
C3 0.0602(13) 0.188(3) 0.0471(11) -0.0073(14) 0.0160(10) -0.0271(15)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl Si1 Si2 105.508(18) . 5 ?
Cl Si1 Si2 105.508(18) . . ?
Si2 Si1 Si2 113.127(15) 5 . ?
Cl Si1 Si2 105.508(18) . 9 ?
Si2 Si1 Si2 113.127(15) 5 9 ?
Si2 Si1 Si2 113.127(15) . 9 ?
C1 Si2 C3 106.81(14) . . ?
C1 Si2 C2 109.77(11) . . ?
C3 Si2 C2 110.17(10) . . ?
C1 Si2 Si1 110.54(8) . . ?
C3 Si2 Si1 110.36(7) . . ?
C2 Si2 Si1 109.17(7) . . ?
Si2 C2 H2A 109.5 . . ?
Si2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si2 C1 H1A 109.5 . . ?
Si2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si2 C3 H3A 109.5 . . ?
Si2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 Cl 2.1248(9) . ?
Si1 Si2 2.3406(6) 5 ?
Si1 Si2 2.3406(6) . ?
Si1 Si2 2.3406(6) 9 ?
Si2 C1 1.860(2) . ?
Si2 C3 1.862(2) . ?
Si2 C2 1.8663(18) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl Si1 Si2 C1 -60.46(10) . . . . ?
Si2 Si1 Si2 C1 54.39(11) 5 . . . ?
Si2 Si1 Si2 C1 -175.31(10) 9 . . . ?
Cl Si1 Si2 C3 57.48(9) . . . . ?
Si2 Si1 Si2 C3 172.32(9) 5 . . . ?
Si2 Si1 Si2 C3 -57.37(10) 9 . . . ?
Cl Si1 Si2 C2 178.69(8) . . . . ?
Si2 Si1 Si2 C2 -66.46(8) 5 . . . ?
Si2 Si1 Si2 C2 63.84(8) 9 . . . ?
