#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/55/2205545.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2205545
loop_
_publ_author_name
'Ferguson, George'
'O'Leary, Brian J.'
'Spalding, Trevor R.'
_publ_section_title
;
 Tris(triphenylsilyl)phosphate dichloromethane solvate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o906
_journal_page_last               o907
_journal_paper_doi               10.1107/S1600536805006604
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C54 H45 O4 P Si3, 0.263C H2 Cl2'
_chemical_formula_moiety         'C54 H45 O4 P Si3, 0.263C H2 Cl2'
_chemical_formula_sum            'C54.26 H45.53 Cl0.53 O4 P Si3'
_chemical_formula_weight         895.48
_chemical_name_systematic
;
Tris(triphenylsilyl)phosphate dichloromethane solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                91.75(2)
_cell_angle_beta                 105.47(2)
_cell_angle_gamma                106.31(2)
_cell_formula_units_Z            2
_cell_length_a                   10.284(2)
_cell_length_b                   13.055(3)
_cell_length_c                   19.015(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.0(10)
_cell_measurement_theta_max      14.00
_cell_measurement_theta_min      6.15
_cell_volume                     2346.0(9)
_computing_cell_refinement       DIFRAC
_computing_data_collection
'DIFRAC with profile analysis (Gabe & White, 1993)'
_computing_data_reduction        'DATRD2 in NRCVAX94 (Gabe et al., 1989)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  SHELXL97
_computing_structure_refinement
'SHELXL97 (Sheldrick, 1997) in WinGX (Version 1.70.01; Farrugia, 1999)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      294.0(10)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Enraf--Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.1786
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10183
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.93
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        3.8
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             938.1
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.856
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         10183
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.856
_refine_ls_R_factor_all          0.1763
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0501P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                4004
_reflns_number_total             10183
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh6381.cif
_cod_data_source_block           I
_cod_database_code               2205545
_cod_database_fobs_code          2205545
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
P1 0.25013(9) 0.22162(7) 0.20407(5) 0.0355(2) Uani d . 1 . . P
Si1 0.37544(10) 0.38255(8) 0.34356(5) 0.0389(3) Uani d . 1 . . Si
Si2 0.35107(10) 0.34472(8) 0.08450(5) 0.0391(3) Uani d . 1 . . Si
Si3 0.36193(9) 0.02775(8) 0.21775(5) 0.0427(3) Uani d D 1 . . Si
O1 0.3275(2) 0.32790(17) 0.25689(11) 0.0412(6) Uani d . 1 . . O
O2 0.2636(2) 0.25299(17) 0.12812(11) 0.0427(6) Uani d . 1 . . O
O3 0.3505(2) 0.15136(17) 0.22721(12) 0.0471(6) Uani d . 1 A . O
O4 0.1060(2) 0.1708(2) 0.20501(14) 0.0590(7) Uani d . 1 . . O
C11 0.2222(4) 0.4069(3) 0.36612(18) 0.0414(9) Uani d . 1 . . C
C12 0.0950(4) 0.3268(3) 0.3546(2) 0.0640(12) Uani d . 1 . . C
H12 0.0842 0.2596 0.3319 0.077 Uiso calc R 1 . . H
C13 -0.0163(4) 0.3436(4) 0.3759(2) 0.0748(14) Uani d . 1 . . C
H13 -0.1007 0.2884 0.3671 0.090 Uiso calc R 1 . . H
C14 -0.0022(5) 0.4409(4) 0.4097(2) 0.0693(13) Uani d . 1 . . C
H14 -0.0765 0.4516 0.4251 0.083 Uiso calc R 1 . . H
C15 0.1205(5) 0.5232(4) 0.4213(2) 0.0661(12) Uani d . 1 . . C
H15 0.1293 0.5902 0.4436 0.079 Uiso calc R 1 . . H
C16 0.2299(4) 0.5059(3) 0.39987(19) 0.0516(10) Uani d . 1 . . C
H16 0.3129 0.5623 0.4080 0.062 Uiso calc R 1 . . H
C21 0.5154(4) 0.5108(3) 0.34759(19) 0.0413(9) Uani d . 1 . . C
C22 0.4906(4) 0.5859(3) 0.2992(2) 0.0549(11) Uani d . 1 . . C
H22 0.4014 0.5735 0.2662 0.066 Uiso calc R 1 . . H
C23 0.5971(5) 0.6790(3) 0.2997(2) 0.0696(13) Uani d . 1 . . C
H23 0.5791 0.7283 0.2670 0.084 Uiso calc R 1 . . H
C24 0.7284(5) 0.6983(4) 0.3481(3) 0.0768(14) Uani d . 1 . . C
H24 0.8004 0.7599 0.3475 0.092 Uiso calc R 1 . . H
C25 0.7539(4) 0.6273(4) 0.3974(3) 0.0721(13) Uani d . 1 . . C
H25 0.8426 0.6418 0.4313 0.087 Uiso calc R 1 . . H
C26 0.6488(4) 0.5339(3) 0.3974(2) 0.0553(11) Uani d . 1 . . C
H26 0.6678 0.4860 0.4310 0.066 Uiso calc R 1 . . H
C31 0.4465(4) 0.2915(3) 0.40531(19) 0.0451(9) Uani d . 1 . . C
C32 0.5500(4) 0.2495(3) 0.3936(2) 0.0655(12) Uani d . 1 . . C
H32 0.5834 0.2662 0.3532 0.079 Uiso calc R 1 . . H
C33 0.6046(5) 0.1833(4) 0.4410(3) 0.0837(15) Uani d . 1 . . C
H33 0.6719 0.1542 0.4315 0.100 Uiso calc R 1 . . H
C34 0.5588(6) 0.1608(4) 0.5020(3) 0.0920(17) Uani d . 1 . . C
H34 0.5960 0.1170 0.5340 0.110 Uiso calc R 1 . . H
C35 0.4595(6) 0.2020(4) 0.5158(3) 0.0905(16) Uani d . 1 . . C
H35 0.4286 0.1868 0.5571 0.109 Uiso calc R 1 . . H
C36 0.4046(4) 0.2672(3) 0.4673(2) 0.0633(12) Uani d . 1 . . C
H36 0.3370 0.2954 0.4772 0.076 Uiso calc R 1 . . H
C41 0.2854(3) 0.2855(3) -0.01307(18) 0.0378(8) Uani d . 1 . . C
C42 0.2848(4) 0.1825(3) -0.0333(2) 0.0550(11) Uani d . 1 . . C
H42 0.3173 0.1419 0.0029 0.066 Uiso calc R 1 . . H
C43 0.2370(5) 0.1386(3) -0.1059(2) 0.0698(13) Uani d . 1 . . C
H43 0.2403 0.0700 -0.1182 0.084 Uiso calc R 1 . . H
C44 0.1848(5) 0.1960(4) -0.1599(2) 0.0732(13) Uani d . 1 . . C
H44 0.1501 0.1660 -0.2087 0.088 Uiso calc R 1 . . H
C45 0.1843(4) 0.2978(4) -0.1413(2) 0.0676(12) Uani d . 1 . . C
H45 0.1503 0.3374 -0.1778 0.081 Uiso calc R 1 . . H
C46 0.2335(4) 0.3423(3) -0.0690(2) 0.0535(10) Uani d . 1 . . C
H46 0.2320 0.4116 -0.0573 0.064 Uiso calc R 1 . . H
C51 0.5447(3) 0.3673(3) 0.12188(19) 0.0385(9) Uani d . 1 . . C
C52 0.6175(4) 0.4158(3) 0.1932(2) 0.0528(10) Uani d . 1 . . C
H52 0.5677 0.4366 0.2224 0.063 Uiso calc R 1 . . H
C53 0.7603(4) 0.4337(3) 0.2217(2) 0.0683(12) Uani d . 1 . . C
H53 0.8057 0.4659 0.2697 0.082 Uiso calc R 1 . . H
C54 0.8363(4) 0.4042(3) 0.1795(3) 0.0654(12) Uani d . 1 . . C
H54 0.9329 0.4150 0.1990 0.078 Uiso calc R 1 . . H
C55 0.7683(4) 0.3585(3) 0.1084(3) 0.0617(12) Uani d . 1 . . C
H55 0.8197 0.3402 0.0791 0.074 Uiso calc R 1 . . H
C56 0.6245(4) 0.3395(3) 0.0802(2) 0.0513(10) Uani d . 1 . . C
H56 0.5798 0.3074 0.0322 0.062 Uiso calc R 1 . . H
C61 0.3015(4) 0.4691(3) 0.09609(18) 0.0388(9) Uani d . 1 . . C
C62 0.1634(4) 0.4630(3) 0.0928(2) 0.0653(12) Uani d . 1 . . C
H62 0.0975 0.3960 0.0888 0.078 Uiso calc R 1 . . H
C63 0.1212(5) 0.5546(4) 0.0954(3) 0.0817(15) Uani d . 1 . . C
H63 0.0278 0.5490 0.0927 0.098 Uiso calc R 1 . . H
C64 0.2186(5) 0.6540(4) 0.1021(2) 0.0690(13) Uani d . 1 . . C
H64 0.1910 0.7158 0.1038 0.083 Uiso calc R 1 . . H
C65 0.3559(5) 0.6619(3) 0.1063(2) 0.0601(11) Uani d . 1 . . C
H65 0.4217 0.7292 0.1112 0.072 Uiso calc R 1 . . H
C66 0.3967(4) 0.5704(3) 0.10317(19) 0.0496(10) Uani d . 1 . . C
H66 0.4904 0.5768 0.1059 0.059 Uiso calc R 1 . . H
C71 0.2619(19) -0.0512(15) 0.2766(9) 0.0525(16) Uani d PGD 0.50 A -1 C
C72 0.2384(16) 0.0034(8) 0.3336(11) 0.072(4) Uani d PG 0.50 A -1 C
H72 0.2704 0.0781 0.3410 0.087 Uiso calc PR 0.50 A -1 H
C73 0.1672(14) -0.0536(7) 0.3797(8) 0.093(4) Uani d PG 0.50 A -1 C
H73 0.1515 -0.0170 0.4178 0.111 Uiso calc PR 0.50 A -1 H
C74 0.1194(15) -0.1652(7) 0.3687(6) 0.086(5) Uani d PG 0.50 A -1 C
H74 0.0718 -0.2033 0.3995 0.103 Uiso calc PR 0.50 A -1 H
C75 0.1429(16) -0.2198(9) 0.3117(7) 0.085(4) Uani d PG 0.50 A -1 C
H75 0.1109 -0.2944 0.3043 0.102 Uiso calc PR 0.50 A -1 H
C76 0.2141(17) -0.1628(15) 0.2656(7) 0.070(4) Uani d PG 0.50 A -1 C
H76 0.2298 -0.1994 0.2275 0.084 Uiso calc PR 0.50 A -1 H
C711 0.2671(19) -0.0617(14) 0.2742(10) 0.0525(16) Uani d PGD 0.50 A -2 C
C721 0.1965(17) -0.0283(8) 0.3191(11) 0.072(4) Uani d PG 0.50 A -2 C
H721 0.2009 0.0437 0.3251 0.087 Uiso calc PR 0.50 A -2 H
C731 0.1193(13) -0.1025(7) 0.3550(8) 0.093(4) Uani d PG 0.50 A -2 C
H731 0.0720 -0.0802 0.3850 0.111 Uiso calc PR 0.50 A -2 H
C741 0.1127(14) -0.2101(7) 0.3460(7) 0.086(5) Uani d PG 0.50 A -2 C
H741 0.0610 -0.2597 0.3700 0.103 Uiso calc PR 0.50 A -2 H
C751 0.1833(15) -0.2435(10) 0.3011(9) 0.085(4) Uani d PG 0.50 A -2 C
H751 0.1789 -0.3154 0.2951 0.102 Uiso calc PR 0.50 A -2 H
C761 0.2605(17) -0.1693(15) 0.2652(8) 0.070(4) Uani d PG 0.50 A -2 C
H761 0.3078 -0.1916 0.2352 0.084 Uiso calc PR 0.50 A -2 H
C81 0.5546(5) 0.0427(17) 0.2489(12) 0.0451(10) Uani d PGD 0.50 A -1 C
C82 0.6412(17) 0.1042(16) 0.2110(10) 0.046(3) Uani d PG 0.50 A -1 C
H82 0.6037 0.1404 0.1732 0.055 Uiso calc PR 0.50 A -1 H
C83 0.7840(15) 0.1116(15) 0.2297(12) 0.058(2) Uani d PG 0.50 A -1 C
H83 0.8420 0.1528 0.2044 0.069 Uiso calc PR 0.50 A -1 H
C84 0.8402(6) 0.0575(17) 0.2862(12) 0.080(2) Uani d PG 0.50 A -1 C
H84 0.9357 0.0625 0.2987 0.096 Uiso calc PR 0.50 A -1 H
C85 0.7535(16) -0.0040(14) 0.3241(9) 0.069(4) Uani d PG 0.50 A -1 C
H85 0.7911 -0.0402 0.3619 0.083 Uiso calc PR 0.50 A -1 H
C86 0.6107(14) -0.0115(14) 0.3054(10) 0.055(3) Uani d PG 0.50 A -1 C
H86 0.5527 -0.0526 0.3307 0.066 Uiso calc PR 0.50 A -1 H
C811 0.5551(5) 0.0443(17) 0.2465(12) 0.0451(10) Uani d PGD 0.50 A -2 C
C821 0.6469(17) 0.1271(15) 0.2233(11) 0.046(3) Uani d PG 0.50 A -2 C
H821 0.6137 0.1792 0.1987 0.055 Uiso calc PR 0.50 A -2 H
C831 0.7883(15) 0.1319(15) 0.2370(12) 0.058(2) Uani d PG 0.50 A -2 C
H831 0.8497 0.1873 0.2215 0.069 Uiso calc PR 0.50 A -2 H
C841 0.8379(6) 0.0540(17) 0.2739(12) 0.080(2) Uani d PG 0.50 A -2 C
H841 0.9325 0.0572 0.2830 0.096 Uiso calc PR 0.50 A -2 H
C851 0.7462(16) -0.0288(14) 0.2971(9) 0.069(4) Uani d PG 0.50 A -2 C
H851 0.7794 -0.0809 0.3218 0.083 Uiso calc PR 0.50 A -2 H
C861 0.6047(14) -0.0337(14) 0.2834(10) 0.055(3) Uani d PG 0.50 A -2 C
H861 0.5433 -0.0891 0.2990 0.066 Uiso calc PR 0.50 A -2 H
C91 0.2855(4) -0.0304(3) 0.1195(2) 0.0443(9) Uani d . 1 A . C
C92 0.1399(4) -0.0575(3) 0.0865(2) 0.0542(10) Uani d . 1 . . C
H92 0.0819 -0.0455 0.1140 0.065 Uiso calc R 1 A . H
C93 0.0805(4) -0.1013(3) 0.0146(2) 0.0653(12) Uani d . 1 A . C
H93 -0.0170 -0.1188 -0.0058 0.078 Uiso calc R 1 . . H
C94 0.1621(5) -0.1196(3) -0.0274(2) 0.0655(12) Uani d . 1 . . C
H94 0.1210 -0.1484 -0.0763 0.079 Uiso calc R 1 A . H
C95 0.3070(5) -0.0949(3) 0.0036(2) 0.0631(11) Uani d . 1 A . C
H95 0.3639 -0.1077 -0.0242 0.076 Uiso calc R 1 . . H
C96 0.3665(4) -0.0507(3) 0.0766(2) 0.0545(10) Uani d . 1 . . C
H96 0.4638 -0.0343 0.0971 0.065 Uiso calc R 1 A . H
Cl1 0.0618(10) 0.1009(11) 0.4839(8) 0.127(3) Uani d P 0.263(2) . . Cl
Cl2 0.0136(10) -0.1147(11) 0.5188(8) 0.127(3) Uani d P 0.263(2) . . Cl
C1 0.128(2) 0.0105(19) 0.5151(12) 0.130(8) Uiso d P 0.263(2) . . C
H1A 0.1891 0.0376 0.5644 0.156 Uiso calc PR 0.263(2) . . H
H1B 0.1877 -0.0002 0.4855 0.156 Uiso calc PR 0.263(2) . . H
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
2 -2 3
-1 1 6
-3 -2 4
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O4 P1 O2 113.92(14) ?
O4 P1 O3 114.22(15) ?
O2 P1 O3 104.90(13) ?
O4 P1 O1 114.68(14) ?
O2 P1 O1 104.40(12) ?
O3 P1 O1 103.52(12) ?
O1 Si1 C11 109.83(14) ?
O1 Si1 C31 109.37(14) ?
C11 Si1 C31 110.59(17) ?
O1 Si1 C21 104.62(14) ?
C11 Si1 C21 111.28(16) ?
C31 Si1 C21 110.97(17) ?
O2 Si2 C61 107.50(14) ?
O2 Si2 C41 104.42(13) ?
C61 Si2 C41 111.07(16) ?
O2 Si2 C51 110.02(14) ?
C61 Si2 C51 112.15(15) ?
C41 Si2 C51 111.32(16) ?
O3 Si3 C711 111.7(7) ?
O3 Si3 C71 106.4(7) ?
O3 Si3 C81 105.2(6) ?
C711 Si3 C81 110.6(10) ?
C71 Si3 C81 113.2(10) ?
O3 Si3 C811 104.8(6) ?
C711 Si3 C811 112.1(10) ?
C71 Si3 C811 114.7(10) ?
O3 Si3 C91 110.07(14) ?
C711 Si3 C91 108.8(7) ?
C71 Si3 C91 111.2(7) ?
C81 Si3 C91 110.4(6) ?
C811 Si3 C91 109.3(6) ?
P1 O1 Si1 144.47(15) y
P1 O2 Si2 144.71(15) y
P1 O3 Si3 143.57(16) y
C12 C11 C16 115.7(3) ?
C12 C11 Si1 122.3(3) ?
C16 C11 Si1 122.0(3) ?
C13 C12 C11 122.0(4) ?
C13 C12 H12 119.0 ?
C11 C12 H12 119.0 ?
C14 C13 C12 119.9(4) ?
C14 C13 H13 120.1 ?
C12 C13 H13 120.1 ?
C13 C14 C15 120.4(4) ?
C13 C14 H14 119.8 ?
C15 C14 H14 119.8 ?
C16 C15 C14 119.3(4) ?
C16 C15 H15 120.4 ?
C14 C15 H15 120.4 ?
C15 C16 C11 122.7(4) ?
C15 C16 H16 118.6 ?
C11 C16 H16 118.6 ?
C26 C21 C22 117.7(3) ?
C26 C21 Si1 121.4(3) ?
C22 C21 Si1 120.9(3) ?
C23 C22 C21 120.9(4) ?
C23 C22 H22 119.5 ?
C21 C22 H22 119.5 ?
C24 C23 C22 120.1(4) ?
C24 C23 H23 120.0 ?
C22 C23 H23 120.0 ?
C23 C24 C25 120.0(4) ?
C23 C24 H24 120.0 ?
C25 C24 H24 120.0 ?
C24 C25 C26 120.5(4) ?
C24 C25 H25 119.7 ?
C26 C25 H25 119.7 ?
C25 C26 C21 120.7(4) ?
C25 C26 H26 119.6 ?
C21 C26 H26 119.6 ?
C36 C31 C32 116.8(4) ?
C36 C31 Si1 121.3(3) ?
C32 C31 Si1 121.8(3) ?
C31 C32 C33 121.4(4) ?
C31 C32 H32 119.3 ?
C33 C32 H32 119.3 ?
C34 C33 C32 119.6(5) ?
C34 C33 H33 120.2 ?
C32 C33 H33 120.2 ?
C35 C34 C33 120.5(5) ?
C35 C34 H34 119.8 ?
C33 C34 H34 119.8 ?
C34 C35 C36 119.1(5) ?
C34 C35 H35 120.4 ?
C36 C35 H35 120.4 ?
C31 C36 C35 122.5(4) ?
C31 C36 H36 118.7 ?
C35 C36 H36 118.7 ?
C42 C41 C46 117.1(3) ?
C42 C41 Si2 121.5(3) ?
C46 C41 Si2 121.4(3) ?
C43 C42 C41 121.6(4) ?
C43 C42 H42 119.2 ?
C41 C42 H42 119.2 ?
C44 C43 C42 120.0(4) ?
C44 C43 H43 120.0 ?
C42 C43 H43 120.0 ?
C45 C44 C43 119.4(4) ?
C45 C44 H44 120.3 ?
C43 C44 H44 120.3 ?
C44 C45 C46 120.7(4) ?
C44 C45 H45 119.7 ?
C46 C45 H45 119.7 ?
C45 C46 C41 121.2(4) ?
C45 C46 H46 119.4 ?
C41 C46 H46 119.4 ?
C56 C51 C52 116.6(3) ?
C56 C51 Si2 122.3(3) ?
C52 C51 Si2 121.1(3) ?
C53 C52 C51 122.0(4) ?
C53 C52 H52 119.0 ?
C51 C52 H52 119.0 ?
C52 C53 C54 120.1(4) ?
C52 C53 H53 120.0 ?
C54 C53 H53 120.0 ?
C55 C54 C53 119.4(4) ?
C55 C54 H54 120.3 ?
C53 C54 H54 120.3 ?
C54 C55 C56 120.4(4) ?
C54 C55 H55 119.8 ?
C56 C55 H55 119.8 ?
C55 C56 C51 121.5(4) ?
C55 C56 H56 119.3 ?
C51 C56 H56 119.3 ?
C66 C61 C62 117.5(3) ?
C66 C61 Si2 122.1(3) ?
C62 C61 Si2 120.2(3) ?
C61 C62 C63 121.3(4) ?
C61 C62 H62 119.3 ?
C63 C62 H62 119.3 ?
C64 C63 C62 119.5(4) ?
C64 C63 H63 120.2 ?
C62 C63 H63 120.2 ?
C65 C64 C63 120.1(4) ?
C65 C64 H64 120.0 ?
C63 C64 H64 120.0 ?
C64 C65 C66 120.0(4) ?
C64 C65 H65 120.0 ?
C66 C65 H65 120.0 ?
C65 C66 C61 121.5(4) ?
C65 C66 H66 119.3 ?
C61 C66 H66 119.3 ?
C72 C71 C76 120.0 ?
C72 C71 Si3 118.7(11) ?
C76 C71 Si3 121.3(11) ?
C71 C72 C73 120.0 ?
C71 C72 H72 120.0 ?
C73 C72 H72 120.0 ?
C74 C73 C72 120.0 ?
C74 C73 H73 120.0 ?
C72 C73 H73 120.0 ?
C75 C74 C73 120.0 ?
C75 C74 H74 120.0 ?
C73 C74 H74 120.0 ?
C74 C75 C76 120.0 ?
C74 C75 H75 120.0 ?
C76 C75 H75 120.0 ?
C75 C76 C71 120.0 ?
C75 C76 H76 120.0 ?
C71 C76 H76 120.0 ?
C721 C711 C761 120.0 ?
C721 C711 Si3 123.9(11) ?
C761 C711 Si3 115.9(11) ?
C731 C721 C711 120.0 ?
C731 C721 H721 120.0 ?
C711 C721 H721 120.0 ?
C721 C731 C741 120.0 ?
C721 C731 H731 120.0 ?
C741 C731 H731 120.0 ?
C751 C741 C731 120.0 ?
C751 C741 H741 120.0 ?
C731 C741 H741 120.0 ?
C761 C751 C741 120.0 ?
C761 C751 H751 120.0 ?
C741 C751 H751 120.0 ?
C751 C761 C711 120.0 ?
C751 C761 H761 120.0 ?
C711 C761 H761 120.0 ?
C82 C81 C86 120.0 ?
C82 C81 Si3 118.4(13) ?
C86 C81 Si3 121.5(13) ?
C81 C82 C83 120.0 ?
C81 C82 H82 120.0 ?
C83 C82 H82 120.0 ?
C84 C83 C82 120.0 ?
C84 C83 H83 120.0 ?
C82 C83 H83 120.0 ?
C83 C84 C85 120.0 ?
C83 C84 H84 120.0 ?
C85 C84 H84 120.0 ?
C84 C85 C86 120.0 ?
C84 C85 H85 120.0 ?
C86 C85 H85 120.0 ?
C85 C86 C81 120.0 ?
C85 C86 H86 120.0 ?
C81 C86 H86 120.0 ?
C821 C811 C861 120.0 ?
C821 C811 Si3 119.8(13) ?
C861 C811 Si3 119.7(13) ?
C831 C821 C811 120.0 ?
C831 C821 H821 120.0 ?
C811 C821 H821 120.0 ?
C821 C831 C841 120.0 ?
C821 C831 H831 120.0 ?
C841 C831 H831 120.0 ?
C851 C841 C831 120.0 ?
C851 C841 H841 120.0 ?
C831 C841 H841 120.0 ?
C861 C851 C841 120.0 ?
C861 C851 H851 120.0 ?
C841 C851 H851 120.0 ?
C851 C861 C811 120.0 ?
C851 C861 H861 120.0 ?
C811 C861 H861 120.0 ?
C96 C91 C92 116.9(4) ?
C96 C91 Si3 122.9(3) ?
C92 C91 Si3 120.1(3) ?
C93 C92 C91 121.5(4) ?
C93 C92 H92 119.3 ?
C91 C92 H92 119.3 ?
C94 C93 C92 120.9(4) ?
C94 C93 H93 119.5 ?
C92 C93 H93 119.5 ?
C93 C94 C95 119.3(4) ?
C93 C94 H94 120.3 ?
C95 C94 H94 120.3 ?
C94 C95 C96 119.4(4) ?
C94 C95 H95 120.3 ?
C96 C95 H95 120.3 ?
C91 C96 C95 121.9(4) ?
C91 C96 H96 119.0 ?
C95 C96 H96 119.0 ?
Cl1 C1 Cl2 118.2(14) ?
Cl1 C1 H1A 107.8 ?
Cl2 C1 H1A 107.8 ?
Cl1 C1 H1B 107.8 ?
Cl2 C1 H1B 107.8 ?
H1A C1 H1B 107.1 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
P1 O1 1.561(2) y
P1 O2 1.544(2) y
P1 O3 1.554(2) y
P1 O4 1.449(2) y
Si1 O1 1.663(2) y
Si1 C11 1.844(3) ?
Si1 C31 1.856(4) ?
Si1 C21 1.860(4) ?
Si2 O2 1.669(2) y
Si2 C61 1.857(3) ?
Si2 C41 1.857(3) ?
Si2 C51 1.860(3) ?
Si3 O3 1.659(2) y
Si3 C711 1.8608(11) ?
Si3 C71 1.8610(11) ?
Si3 C81 1.8612(11) ?
Si3 C811 1.8613(11) ?
Si3 C91 1.865(4) ?
C11 C12 1.385(5) ?
C11 C16 1.398(5) ?
C12 C13 1.380(5) ?
C12 H12 0.93 ?
C13 C14 1.358(5) ?
C13 H13 0.93 ?
C14 C15 1.367(5) ?
C14 H14 0.93 ?
C15 C16 1.366(5) ?
C15 H15 0.93 ?
C16 H16 0.93 ?
C21 C26 1.388(5) ?
C21 C22 1.394(5) ?
C22 C23 1.386(5) ?
C22 H22 0.93 ?
C23 C24 1.366(6) ?
C23 H23 0.93 ?
C24 C25 1.367(6) ?
C24 H24 0.93 ?
C25 C26 1.383(5) ?
C25 H25 0.93 ?
C26 H26 0.93 ?
C31 C36 1.376(5) ?
C31 C32 1.388(5) ?
C32 C33 1.387(6) ?
C32 H32 0.93 ?
C33 C34 1.374(6) ?
C33 H33 0.93 ?
C34 C35 1.358(6) ?
C34 H34 0.93 ?
C35 C36 1.390(5) ?
C35 H35 0.93 ?
C36 H36 0.93 ?
C41 C42 1.385(4) ?
C41 C46 1.390(5) ?
C42 C43 1.381(5) ?
C42 H42 0.93 ?
C43 C44 1.373(5) ?
C43 H43 0.93 ?
C44 C45 1.366(5) ?
C44 H44 0.93 ?
C45 C46 1.378(5) ?
C45 H45 0.93 ?
C46 H46 0.93 ?
C51 C56 1.389(4) ?
C51 C52 1.393(5) ?
C52 C53 1.371(5) ?
C52 H52 0.93 ?
C53 C54 1.374(5) ?
C53 H53 0.93 ?
C54 C55 1.373(5) ?
C54 H54 0.93 ?
C55 C56 1.379(5) ?
C55 H55 0.93 ?
C56 H56 0.93 ?
C61 C66 1.384(4) ?
C61 C62 1.385(4) ?
C62 C63 1.386(5) ?
C62 H62 0.93 ?
C63 C64 1.377(5) ?
C63 H63 0.93 ?
C64 C65 1.366(5) ?
C64 H64 0.93 ?
C65 C66 1.379(5) ?
C65 H65 0.93 ?
C66 H66 0.93 ?
C71 C72 1.39 ?
C71 C76 1.39 ?
C72 C73 1.39 ?
C72 H72 0.93 ?
C73 C74 1.39 ?
C73 H73 0.93 ?
C74 C75 1.39 ?
C74 H74 0.93 ?
C75 C76 1.39 ?
C75 H75 0.93 ?
C76 H76 0.93 ?
C711 C721 1.39 ?
C711 C761 1.39 ?
C721 C731 1.39 ?
C721 H721 0.93 ?
C731 C741 1.39 ?
C731 H731 0.93 ?
C741 C751 1.39 ?
C741 H741 0.93 ?
C751 C761 1.39 ?
C751 H751 0.93 ?
C761 H761 0.93 ?
C81 C82 1.39 ?
C81 C86 1.39 ?
C82 C83 1.39 ?
C82 H82 0.93 ?
C83 C84 1.39 ?
C83 H83 0.93 ?
C84 C85 1.39 ?
C84 H84 0.93 ?
C85 C86 1.39 ?
C85 H85 0.93 ?
C86 H86 0.93 ?
C811 C821 1.39 ?
C811 C861 1.39 ?
C821 C831 1.39 ?
C821 H821 0.93 ?
C831 C841 1.39 ?
C831 H831 0.93 ?
C841 C851 1.39 ?
C841 H841 0.93 ?
C851 C861 1.39 ?
C851 H851 0.93 ?
C861 H861 0.93 ?
C91 C96 1.380(5) ?
C91 C92 1.395(5) ?
C92 C93 1.373(5) ?
C92 H92 0.93 ?
C93 C94 1.362(5) ?
C93 H93 0.93 ?
C94 C95 1.386(5) ?
C94 H94 0.93 ?
C95 C96 1.390(5) ?
C95 H95 0.93 ?
C96 H96 0.93 ?
Cl1 C1 1.58(3) ?
Cl2 C1 1.74(3) ?
C1 H1A 0.97 ?
C1 H1B 0.97 ?
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
O4 P1 O1 Si1 55.8(3)
O2 P1 O1 Si1 -178.9(2)
O3 P1 O1 Si1 -69.3(3)
C11 Si1 O1 P1 -77.8(3)
C31 Si1 O1 P1 43.7(3)
C21 Si1 O1 P1 162.6(3)
O4 P1 O2 Si2 143.5(3)
O3 P1 O2 Si2 -90.9(3)
O1 P1 O2 Si2 17.6(3)
C61 Si2 O2 P1 -69.0(3)
C41 Si2 O2 P1 173.0(3)
C51 Si2 O2 P1 53.4(3)
O4 P1 O3 Si3 42.3(3)
O2 P1 O3 Si3 -83.1(3)
O1 P1 O3 Si3 167.7(2)
C711 Si3 O3 P1 -76.6(7)
C71 Si3 O3 P1 -76.3(7)
C81 Si3 O3 P1 163.3(8)
C811 Si3 O3 P1 161.8(8)
C91 Si3 O3 P1 44.4(3)
O1 Si1 C11 C12 53.1(3)
C31 Si1 C11 C12 -67.7(3)
C21 Si1 C11 C12 168.5(3)
O1 Si1 C11 C16 -130.6(3)
C31 Si1 C11 C16 108.5(3)
C21 Si1 C11 C16 -15.3(3)
C16 C11 C12 C13 -0.7(6)
Si1 C11 C12 C13 175.8(3)
C11 C12 C13 C14 -0.5(7)
C12 C13 C14 C15 1.5(7)
C13 C14 C15 C16 -1.3(6)
C14 C15 C16 C11 0.1(6)
C12 C11 C16 C15 0.9(5)
Si1 C11 C16 C15 -175.6(3)
O1 Si1 C21 C26 -124.0(3)
C11 Si1 C21 C26 117.5(3)
C31 Si1 C21 C26 -6.2(3)
O1 Si1 C21 C22 54.3(3)
C11 Si1 C21 C22 -64.3(3)
C31 Si1 C21 C22 172.1(3)
C26 C21 C22 C23 1.7(5)
Si1 C21 C22 C23 -176.7(3)
C21 C22 C23 C24 -0.1(6)
C22 C23 C24 C25 -1.7(7)
C23 C24 C25 C26 2.0(7)
C24 C25 C26 C21 -0.4(6)
C22 C21 C26 C25 -1.4(5)
Si1 C21 C26 C25 176.9(3)
O1 Si1 C31 C36 -133.3(3)
C11 Si1 C31 C36 -12.2(4)
C21 Si1 C31 C36 111.8(3)
O1 Si1 C31 C32 50.4(3)
C11 Si1 C31 C32 171.5(3)
C21 Si1 C31 C32 -64.5(3)
C36 C31 C32 C33 2.2(6)
Si1 C31 C32 C33 178.6(3)
C31 C32 C33 C34 -1.9(7)
C32 C33 C34 C35 0.7(8)
C33 C34 C35 C36 0.1(8)
C32 C31 C36 C35 -1.4(6)
Si1 C31 C36 C35 -177.9(3)
C34 C35 C36 C31 0.3(7)
O2 Si2 C41 C42 -51.6(3)
C61 Si2 C41 C42 -167.2(3)
C51 Si2 C41 C42 67.1(3)
O2 Si2 C41 C46 127.8(3)
C61 Si2 C41 C46 12.2(3)
C51 Si2 C41 C46 -113.6(3)
C46 C41 C42 C43 1.1(6)
Si2 C41 C42 C43 -179.5(3)
C41 C42 C43 C44 -1.9(6)
C42 C43 C44 C45 1.8(7)
C43 C44 C45 C46 -1.0(7)
C44 C45 C46 C41 0.2(6)
C42 C41 C46 C45 -0.3(5)
Si2 C41 C46 C45 -179.7(3)
O2 Si2 C51 C56 113.9(3)
C61 Si2 C51 C56 -126.5(3)
C41 Si2 C51 C56 -1.4(3)
O2 Si2 C51 C52 -67.7(3)
C61 Si2 C51 C52 51.9(3)
C41 Si2 C51 C52 177.0(3)
C56 C51 C52 C53 -1.1(6)
Si2 C51 C52 C53 -179.6(3)
C51 C52 C53 C54 0.3(6)
C52 C53 C54 C55 1.2(6)
C53 C54 C55 C56 -1.9(6)
C54 C55 C56 C51 1.1(6)
C52 C51 C56 C55 0.4(5)
Si2 C51 C56 C55 178.9(3)
O2 Si2 C61 C66 145.2(3)
C41 Si2 C61 C66 -101.1(3)
C51 Si2 C61 C66 24.2(3)
O2 Si2 C61 C62 -39.3(3)
C41 Si2 C61 C62 74.4(3)
C51 Si2 C61 C62 -160.3(3)
C66 C61 C62 C63 0.9(6)
Si2 C61 C62 C63 -174.8(3)
C61 C62 C63 C64 -0.6(7)
C62 C63 C64 C65 -0.1(7)
C63 C64 C65 C66 0.5(7)
C64 C65 C66 C61 -0.2(6)
C62 C61 C66 C65 -0.5(5)
Si2 C61 C66 C65 175.1(3)
O3 Si3 C71 C72 -21.1(10)
C711 Si3 C71 C72 155(15)
C81 Si3 C71 C72 94.0(11)
C811 Si3 C71 C72 94.3(11)
C91 Si3 C71 C72 -141.0(7)
O3 Si3 C71 C76 160.6(8)
C711 Si3 C71 C76 -23(13)
C81 Si3 C71 C76 -84.3(11)
C811 Si3 C71 C76 -84.1(12)
C91 Si3 C71 C76 40.7(10)
Si3 C71 C72 C73 -178.4(14)
Si3 C71 C76 C75 178.3(14)
O3 Si3 C711 C721 -0.5(11)
C71 Si3 C711 C721 -4(13)
C81 Si3 C711 C721 116.4(10)
C811 Si3 C711 C721 116.8(10)
C91 Si3 C711 C721 -122.2(8)
O3 Si3 C711 C761 174.8(7)
C71 Si3 C711 C761 171(15)
C81 Si3 C711 C761 -68.4(11)
C811 Si3 C711 C761 -68.0(11)
C91 Si3 C711 C761 53.1(9)
Si3 C711 C721 C731 175.0(14)
Si3 C711 C761 C751 -175.4(13)
O3 Si3 C81 C82 -61.3(7)
C711 Si3 C81 C82 177.9(9)
C71 Si3 C81 C82 -177.2(9)
C811 Si3 C81 C82 1E1(4)
C91 Si3 C81 C82 57.4(8)
O3 Si3 C81 C86 122.8(7)
C711 Si3 C81 C86 2.0(11)
C71 Si3 C81 C86 6.9(12)
C811 Si3 C81 C86 -17E1(4)
C91 Si3 C81 C86 -118.5(7)
Si3 C81 C82 C83 -176.0(11)
Si3 C81 C86 C85 175.8(11)
O3 Si3 C811 C821 -43.2(8)
C711 Si3 C811 C821 -164.4(9)
C71 Si3 C811 C821 -159.5(9)
C81 Si3 C811 C821 -15E1(4)
C91 Si3 C811 C821 74.8(8)
O3 Si3 C811 C861 144.7(6)
C711 Si3 C811 C861 23.5(12)
C71 Si3 C811 C861 28.4(12)
C81 Si3 C811 C861 4E1(4)
C91 Si3 C811 C861 -97.3(8)
Si3 C811 C821 C831 -172.1(12)
Si3 C811 C861 C851 172.1(12)
O3 Si3 C91 C96 111.3(3)
C711 Si3 C91 C96 -126.0(7)
C71 Si3 C91 C96 -131.0(8)
C81 Si3 C91 C96 -4.4(9)
C811 Si3 C91 C96 -3.3(9)
O3 Si3 C91 C92 -70.0(3)
C711 Si3 C91 C92 52.7(7)
C71 Si3 C91 C92 47.8(8)
C81 Si3 C91 C92 174.3(9)
C811 Si3 C91 C92 175.5(8)
C96 C91 C92 C93 -0.6(5)
Si3 C91 C92 C93 -179.4(3)
C91 C92 C93 C94 -0.3(6)
C92 C93 C94 C95 0.9(6)
C93 C94 C95 C96 -0.8(6)
C92 C91 C96 C95 0.7(5)
Si3 C91 C96 C95 179.5(3)
C94 C95 C96 C91 -0.1(6)
