#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:44:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179861 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/57/7015783.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_7015783
loop_
_publ_author_name
'Kovalenko, Oleksandr O.'
'Brusylovets, Oleksii A.'
'Kinzhybalo, Vasyl'
'Lis, Tadeusz'
'Brusilovets, Anatolii I.'
_publ_section_title
;
 Reactions of ((i)PrO)3M≡M(O(i)Pr)3 (M = Mo, W) with low-coordinate
 phosphorus compounds. Formation of the first four-membered planar
 metallacycles, containing an M≡M triple bond.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4814
_journal_page_last               4817
_journal_paper_doi               10.1039/c1dt10099h
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C27 H69 N2 O6 P Si3 W2'
_chemical_formula_weight         1000.78
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.88(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.679(3)
_cell_length_b                   16.861(4)
_cell_length_c                   21.651(6)
_cell_measurement_reflns_used    31714
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33
_cell_measurement_theta_min      3
_cell_volume                     4200.3(19)
_computing_cell_refinement       'CrysAlisRED (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlisCCD (Oxford Diffraction, 2003)'
_computing_data_reduction        CrysAlisRED
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Kuma KM-4 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            64307
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    5.631
_exptl_absorpt_correction_T_max  0.374
_exptl_absorpt_correction_T_min  0.272
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED (Oxford Diffraction,
2003), analytical numeric
absorption using a multifaceted
crystal model
;
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.87
_refine_diff_density_min         -0.78
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         15009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0196
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0264P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0420
_refine_ls_wR_factor_ref         0.0448
_reflns_number_gt                12588
_reflns_number_total             15009
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10099h.txt
_cod_data_source_block           anat11pa
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7015783
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-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
W1 W 0.462558(6) 0.822781(4) 0.763790(3) 0.01356(2) Uani 1 1 d . . .
W2 W 0.583226(6) 0.710992(4) 0.779977(3) 0.01432(2) Uani 1 1 d . . .
P P 0.45464(4) 0.75831(3) 0.86999(2) 0.01481(8) Uani 1 1 d . . .
N1 N 0.54430(14) 0.68274(9) 0.86364(7) 0.0163(3) Uani 1 1 d . . .
Si1 Si 0.61963(5) 0.60988(3) 0.91301(2) 0.02027(10) Uani 1 1 d . . .
C1 C 0.5743(2) 0.50859(12) 0.88371(11) 0.0318(5) Uani 1 1 d . . .
H1A H 0.4929 0.4997 0.8876 0.048 Uiso 1 1 calc R . .
H1B H 0.6234 0.4689 0.9086 0.048 Uiso 1 1 calc R . .
H1C H 0.5828 0.5040 0.8396 0.048 Uiso 1 1 calc R . .
C2 C 0.5916(2) 0.62296(13) 0.99453(10) 0.0295(4) Uani 1 1 d . . .
H2A H 0.5079 0.6192 0.9947 0.044 Uiso 1 1 calc R . .
H2B H 0.6198 0.6751 1.0103 0.044 Uiso 1 1 calc R . .
H2C H 0.6322 0.5814 1.0215 0.044 Uiso 1 1 calc R . .
C3 C 0.77706(18) 0.61946(14) 0.90873(10) 0.0287(4) Uani 1 1 d . . .
H3A H 0.8042 0.6726 0.9226 0.043 Uiso 1 1 calc R . .
H3B H 0.7885 0.6112 0.8654 0.043 Uiso 1 1 calc R . .
H3C H 0.8213 0.5796 0.9359 0.043 Uiso 1 1 calc R . .
N2 N 0.33049(14) 0.72432(9) 0.89201(7) 0.0181(3) Uani 1 1 d . . .
O1 O 0.30944(11) 0.77894(8) 0.73582(6) 0.0192(3) Uani 1 1 d . . .
C10 C 0.15968(19) 0.87520(13) 0.74562(11) 0.0293(4) Uani 1 1 d . . .
H10A H 0.2170 0.9098 0.7708 0.044 Uiso 1 1 calc R . .
H10B H 0.1260 0.8395 0.7734 0.044 Uiso 1 1 calc R . .
H10C H 0.0980 0.9076 0.7215 0.044 Uiso 1 1 calc R . .
C11 C 0.21861(16) 0.82670(12) 0.70095(9) 0.0217(4) Uani 1 1 d . . .
H11 H 0.2539 0.8638 0.6734 0.026 Uiso 1 1 calc R . .
C12 C 0.13554(19) 0.77182(16) 0.65988(10) 0.0320(5) Uani 1 1 d . . .
H12A H 0.1781 0.7414 0.6326 0.048 Uiso 1 1 calc R . .
H12B H 0.0746 0.8032 0.6341 0.048 Uiso 1 1 calc R . .
H12C H 0.1001 0.7353 0.6863 0.048 Uiso 1 1 calc R . .
O2 O 0.46158(11) 0.87584(8) 0.68415(6) 0.0202(3) Uani 1 1 d . . .
C13 C 0.4165(2) 0.83841(14) 0.57568(10) 0.0288(4) Uani 1 1 d . . .
H13A H 0.3705 0.7943 0.5879 0.043 Uiso 1 1 calc R . .
H13B H 0.4515 0.8226 0.5395 0.043 Uiso 1 1 calc R . .
H13C H 0.3659 0.8844 0.5645 0.043 Uiso 1 1 calc R . .
C14 C 0.51177(17) 0.85990(13) 0.63014(9) 0.0234(4) Uani 1 1 d . . .
H14 H 0.5664 0.8141 0.6392 0.028 Uiso 1 1 calc R . .
C15 C 0.5791(2) 0.93194(16) 0.61494(12) 0.0395(6) Uani 1 1 d . . .
H15A H 0.6388 0.9451 0.6511 0.059 Uiso 1 1 calc R . .
H15B H 0.5259 0.9769 0.6052 0.059 Uiso 1 1 calc R . .
H15C H 0.6163 0.9204 0.5787 0.059 Uiso 1 1 calc R . .
O3 O 0.55696(12) 0.90714(8) 0.80763(6) 0.0195(3) Uani 1 1 d . . .
C16 C 0.4609(3) 1.02638(15) 0.83415(12) 0.0413(6) Uani 1 1 d . . .
H16A H 0.3868 0.9979 0.8284 0.062 Uiso 1 1 calc R . .
H16B H 0.4469 1.0822 0.8226 0.062 Uiso 1 1 calc R . .
H16C H 0.4986 1.0229 0.8781 0.062 Uiso 1 1 calc R . .
C17 C 0.53862(19) 0.98977(11) 0.79308(10) 0.0245(4) Uani 1 1 d . . .
H17 H 0.4996 0.9946 0.7484 0.029 Uiso 1 1 calc R . .
C18 C 0.6549(3) 1.02971(16) 0.8002(2) 0.0689(11) Uani 1 1 d . . .
H18A H 0.7027 1.0034 0.7732 0.103 Uiso 1 1 calc R . .
H18B H 0.6938 1.0262 0.8440 0.103 Uiso 1 1 calc R . .
H18C H 0.6443 1.0856 0.7881 0.103 Uiso 1 1 calc R . .
O4 O 0.54198(12) 0.63773(8) 0.71445(6) 0.0197(3) Uani 1 1 d . . .
C19 C 0.4060(2) 0.55508(14) 0.64706(11) 0.0341(5) Uani 1 1 d . . .
H19A H 0.3554 0.5525 0.6787 0.051 Uiso 1 1 calc R . .
H19B H 0.4613 0.5109 0.6532 0.051 Uiso 1 1 calc R . .
H19C H 0.3587 0.5515 0.6051 0.051 Uiso 1 1 calc R . .
C20 C 0.47181(17) 0.63275(12) 0.65333(9) 0.0219(4) Uani 1 1 d . . .
H20 H 0.4151 0.6777 0.6477 0.026 Uiso 1 1 calc R . .
C21 C 0.5498(2) 0.63889(16) 0.60435(10) 0.0357(5) Uani 1 1 d . . .
H21A H 0.5942 0.6884 0.6104 0.054 Uiso 1 1 calc R . .
H21B H 0.5021 0.6384 0.5624 0.054 Uiso 1 1 calc R . .
H21C H 0.6035 0.5938 0.6086 0.054 Uiso 1 1 calc R . .
O5 O 0.73336(11) 0.75027(8) 0.77869(6) 0.0209(3) Uani 1 1 d . . .
C22 C 0.86823(19) 0.85758(15) 0.80612(11) 0.0331(5) Uani 1 1 d . . .
H22A H 0.8289 0.8744 0.8404 0.050 Uiso 1 1 calc R . .
H22B H 0.9036 0.9038 0.7894 0.050 Uiso 1 1 calc R . .
H22C H 0.9288 0.8188 0.8219 0.050 Uiso 1 1 calc R . .
C23 C 0.78095(17) 0.82020(12) 0.75473(10) 0.0230(4) Uani 1 1 d . . .
H23 H 0.7168 0.8588 0.7407 0.028 Uiso 1 1 calc R . .
C24 C 0.8348(2) 0.79553(14) 0.69871(11) 0.0316(5) Uani 1 1 d . . .
H24A H 0.7751 0.7717 0.6668 0.047 Uiso 1 1 calc R . .
H24B H 0.8966 0.7567 0.7120 0.047 Uiso 1 1 calc R . .
H24C H 0.8676 0.8422 0.6812 0.047 Uiso 1 1 calc R . .
Si2 Si 0.25118(5) 0.64119(3) 0.85774(3) 0.02075(10) Uani 1 1 d . . .
C4 C 0.31211(18) 0.59842(12) 0.79135(10) 0.0253(4) Uani 1 1 d . . .
H4A H 0.3122 0.6389 0.7589 0.038 Uiso 1 1 calc R . .
H4B H 0.2644 0.5533 0.7738 0.038 Uiso 1 1 calc R . .
H4C H 0.3919 0.5805 0.8063 0.038 Uiso 1 1 calc R . .
C5 C 0.09634(18) 0.66388(13) 0.82333(11) 0.0274(4) Uani 1 1 d . . .
H5A H 0.0489 0.6628 0.8565 0.041 Uiso 1 1 calc R . .
H5B H 0.0674 0.6241 0.7914 0.041 Uiso 1 1 calc R . .
H5C H 0.0917 0.7166 0.8041 0.041 Uiso 1 1 calc R . .
C6 C 0.2523(2) 0.56346(14) 0.91925(12) 0.0350(5) Uani 1 1 d . . .
H6A H 0.2099 0.5828 0.9516 0.052 Uiso 1 1 calc R . .
H6B H 0.3327 0.5515 0.9383 0.052 Uiso 1 1 calc R . .
H6C H 0.2147 0.5153 0.9002 0.052 Uiso 1 1 calc R . .
Si3 Si 0.27649(5) 0.77888(3) 0.95130(3) 0.02249(11) Uani 1 1 d . . .
C7 C 0.2718(2) 0.88734(13) 0.93363(10) 0.0303(5) Uani 1 1 d . . .
H7A H 0.3499 0.9058 0.9300 0.045 Uiso 1 1 calc R . .
H7B H 0.2442 0.9161 0.9675 0.045 Uiso 1 1 calc R . .
H7C H 0.2189 0.8970 0.8941 0.045 Uiso 1 1 calc R . .
C8 C 0.1210(2) 0.75360(17) 0.95429(11) 0.0364(5) Uani 1 1 d . . .
H8A H 0.1139 0.6964 0.9606 0.055 Uiso 1 1 calc R . .
H8B H 0.0720 0.7691 0.9148 0.055 Uiso 1 1 calc R . .
H8C H 0.0959 0.7821 0.9891 0.055 Uiso 1 1 calc R . .
C9 C 0.3531(2) 0.75529(15) 1.03225(9) 0.0324(5) Uani 1 1 d . . .
H9A H 0.3400 0.6995 1.0417 0.049 Uiso 1 1 calc R . .
H9B H 0.3228 0.7892 1.0625 0.049 Uiso 1 1 calc R . .
H9C H 0.4366 0.7648 1.0350 0.049 Uiso 1 1 calc R . .
O6 O 0.50606(12) 0.79961(8) 0.93685(6) 0.0196(3) Uani 1 1 d . . .
C25 C 0.7128(2) 0.82971(16) 0.94661(12) 0.0374(6) Uani 1 1 d . . .
H25A H 0.7151 0.8057 0.9056 0.056 Uiso 1 1 calc R . .
H25B H 0.7318 0.7895 0.9795 0.056 Uiso 1 1 calc R . .
H25C H 0.7696 0.8729 0.9540 0.056 Uiso 1 1 calc R . .
C26 C 0.59301(19) 0.86199(12) 0.94773(9) 0.0249(4) Uani 1 1 d . . .
H26 H 0.5743 0.9036 0.9147 0.030 Uiso 1 1 calc R . .
C27 C 0.5848(2) 0.89749(15) 1.01124(11) 0.0364(5) Uani 1 1 d . . .
H27A H 0.5050 0.9155 1.0114 0.055 Uiso 1 1 calc R . .
H27B H 0.6380 0.9426 1.0194 0.055 Uiso 1 1 calc R . .
H27C H 0.6059 0.8573 1.0439 0.055 Uiso 1 1 calc R . .
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'
N N 0.0061 0.0033 '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'
Si Si 0.0817 0.0704 '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'
W W -0.8490 6.8722 '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
O1 W1 O2 91.94(6) . . ?
O1 W1 O3 148.10(6) . . ?
O2 W1 O3 90.74(6) . . ?
O1 W1 W2 103.85(4) . . ?
O2 W1 W2 114.54(4) . . ?
O3 W1 W2 103.84(5) . . ?
O1 W1 P 86.84(5) . . ?
O2 W1 P 176.70(4) . . ?
O3 W1 P 88.68(4) . . ?
W2 W1 P 68.75(2) . . ?
O5 W2 O4 109.83(6) . . ?
O5 W2 N1 117.08(7) . . ?
O4 W2 N1 117.28(6) . . ?
O5 W2 W1 104.66(5) . . ?
O4 W2 W1 110.24(5) . . ?
N1 W2 W1 95.90(5) . . ?
O5 W2 P 121.88(5) . . ?
O4 W2 P 128.28(4) . . ?
N1 W2 P 36.61(5) . . ?
W1 W2 P 59.308(16) . . ?
O6 P N1 105.02(8) . . ?
O6 P N2 95.57(8) . . ?
N1 P N2 110.04(8) . . ?
O6 P W1 123.59(6) . . ?
N1 P W1 97.48(6) . . ?
N2 P W1 123.96(6) . . ?
O6 P W2 125.95(6) . . ?
N1 P W2 45.57(5) . . ?
N2 P W2 133.64(6) . . ?
W1 P W2 51.943(18) . . ?
P N1 Si1 137.48(10) . . ?
P N1 W2 97.82(7) . . ?
Si1 N1 W2 123.26(8) . . ?
N1 Si1 C2 109.98(9) . . ?
N1 Si1 C3 107.68(9) . . ?
C2 Si1 C3 111.86(11) . . ?
N1 Si1 C1 110.42(9) . . ?
C2 Si1 C1 110.16(11) . . ?
C3 Si1 C1 106.67(11) . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
P N2 Si2 123.96(9) . . ?
P N2 Si3 116.89(9) . . ?
Si2 N2 Si3 119.11(9) . . ?
C11 O1 W1 120.63(12) . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O1 C11 C12 107.86(17) . . ?
O1 C11 C10 109.94(16) . . ?
C12 C11 C10 112.85(17) . . ?
O1 C11 H11 108.7 . . ?
C12 C11 H11 108.7 . . ?
C10 C11 H11 108.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 O2 W1 134.72(12) . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O2 C14 C15 109.30(19) . . ?
O2 C14 C13 109.45(16) . . ?
C15 C14 C13 111.18(18) . . ?
O2 C14 H14 109.0 . . ?
C15 C14 H14 109.0 . . ?
C13 C14 H14 109.0 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 O3 W1 123.49(12) . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O3 C17 C18 108.34(19) . . ?
O3 C17 C16 110.49(17) . . ?
C18 C17 C16 112.4(2) . . ?
O3 C17 H17 108.5 . . ?
C18 C17 H17 108.5 . . ?
C16 C17 H17 108.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 O4 W2 140.02(12) . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O4 C20 C19 109.54(17) . . ?
O4 C20 C21 108.94(17) . . ?
C19 C20 C21 110.70(18) . . ?
O4 C20 H20 109.2 . . ?
C19 C20 H20 109.2 . . ?
C21 C20 H20 109.2 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 O5 W2 135.55(12) . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O5 C23 C22 109.27(17) . . ?
O5 C23 C24 107.61(17) . . ?
C22 C23 C24 112.51(18) . . ?
O5 C23 H23 109.1 . . ?
C22 C23 H23 109.1 . . ?
C24 C23 H23 109.1 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N2 Si2 C4 112.93(9) . . ?
N2 Si2 C6 108.52(10) . . ?
C4 Si2 C6 108.85(11) . . ?
N2 Si2 C5 113.87(9) . . ?
C4 Si2 C5 104.10(10) . . ?
C6 Si2 C5 108.36(11) . . ?
Si2 C4 H4A 109.5 . . ?
Si2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 Si3 C7 111.09(9) . . ?
N2 Si3 C9 113.24(9) . . ?
C7 Si3 C9 113.15(11) . . ?
N2 Si3 C8 111.84(10) . . ?
C7 Si3 C8 103.59(12) . . ?
C9 Si3 C8 103.27(11) . . ?
Si3 C7 H7A 109.5 . . ?
Si3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si3 C8 H8A 109.5 . . ?
Si3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si3 C9 H9A 109.5 . . ?
Si3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C26 O6 P 126.56(12) . . ?
C26 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C26 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O6 C26 C25 111.19(17) . . ?
O6 C26 C27 106.33(18) . . ?
C25 C26 C27 111.15(18) . . ?
O6 C26 H26 109.4 . . ?
C25 C26 H26 109.4 . . ?
C27 C26 H26 109.4 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 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
W1 O1 1.9337(14) . ?
W1 O2 1.9409(13) . ?
W1 O3 1.9444(14) . ?
W1 W2 2.3435(4) . ?
W1 P 2.5594(7) . ?
W2 O5 1.8791(14) . ?
W2 O4 1.8805(13) . ?
W2 N1 1.9993(16) . ?
W2 P 2.7739(9) . ?
P O6 1.6257(14) . ?
P N1 1.6699(16) . ?
P N2 1.7015(17) . ?
N1 Si1 1.7615(16) . ?
Si1 C2 1.863(2) . ?
Si1 C3 1.864(2) . ?
Si1 C1 1.867(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
N2 Si2 1.7712(17) . ?
N2 Si3 1.7804(17) . ?
O1 C11 1.438(2) . ?
C10 C11 1.519(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.514(3) . ?
C11 H11 1.0000 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
O2 C14 1.421(2) . ?
C13 C14 1.520(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.514(3) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O3 C17 1.436(2) . ?
C16 C17 1.507(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.500(3) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
O4 C20 1.435(2) . ?
C19 C20 1.513(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.515(3) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
O5 C23 1.438(2) . ?
C22 C23 1.512(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.517(3) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
Si2 C4 1.856(2) . ?
Si2 C6 1.867(2) . ?
Si2 C5 1.873(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
Si3 C7 1.867(2) . ?
Si3 C9 1.869(2) . ?
Si3 C8 1.877(2) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
O6 C26 1.453(2) . ?
C25 C26 1.506(3) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.518(3) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C4 H4A O1 0.98 2.41 3.271(3) 145.9 .
C9 H9C O6 0.98 2.47 3.047(3) 117.2 .
C11 H11 O2 1.00 2.41 3.037(2) 120.5 .
C17 H17 O2 1.00 2.43 3.055(3) 119.6 .
C26 H26 O3 1.00 2.29 3.085(3) 135.4 .
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
O1 W1 W2 O5 160.36(6) . . . . ?
O2 W1 W2 O5 61.68(7) . . . . ?
O3 W1 W2 O5 -35.62(6) . . . . ?
P W1 W2 O5 -118.66(5) . . . . ?
O1 W1 W2 O4 42.32(6) . . . . ?
O2 W1 W2 O4 -56.36(6) . . . . ?
O3 W1 W2 O4 -153.66(6) . . . . ?
P W1 W2 O4 123.30(5) . . . . ?
O1 W1 W2 N1 -79.63(6) . . . . ?
O2 W1 W2 N1 -178.31(6) . . . . ?
O3 W1 W2 N1 84.38(6) . . . . ?
P W1 W2 N1 1.35(5) . . . . ?
O1 W1 W2 P -80.98(5) . . . . ?
O2 W1 W2 P -179.66(5) . . . . ?
O3 W1 W2 P 83.04(5) . . . . ?
O1 W1 P O6 -141.79(8) . . . . ?
O3 W1 P O6 6.61(7) . . . . ?
W2 W1 P O6 112.02(7) . . . . ?
O1 W1 P N1 104.57(7) . . . . ?
O3 W1 P N1 -107.03(7) . . . . ?
W2 W1 P N1 -1.62(6) . . . . ?
O1 W1 P N2 -15.77(8) . . . . ?
O3 W1 P N2 132.63(8) . . . . ?
W2 W1 P N2 -121.96(7) . . . . ?
O1 W1 P W2 106.19(4) . . . . ?
O3 W1 P W2 -105.41(4) . . . . ?
O5 W2 P O6 -18.77(8) . . . . ?
O4 W2 P O6 160.01(8) . . . . ?
N1 W2 P O6 74.77(10) . . . . ?
W1 W2 P O6 -107.47(7) . . . . ?
O5 W2 P N1 -93.55(9) . . . . ?
O4 W2 P N1 85.23(10) . . . . ?
W1 W2 P N1 177.75(8) . . . . ?
O5 W2 P N2 -167.77(9) . . . . ?
O4 W2 P N2 11.01(10) . . . . ?
N1 W2 P N2 -74.23(11) . . . . ?
W1 W2 P N2 103.53(8) . . . . ?
O5 W2 P W1 88.70(6) . . . . ?
O4 W2 P W1 -92.52(6) . . . . ?
N1 W2 P W1 -177.75(8) . . . . ?
O6 P N1 Si1 39.67(16) . . . . ?
N2 P N1 Si1 -62.15(16) . . . . ?
W1 P N1 Si1 167.48(13) . . . . ?
W2 P N1 Si1 165.69(19) . . . . ?
O6 P N1 W2 -126.02(7) . . . . ?
N2 P N1 W2 132.15(8) . . . . ?
W1 P N1 W2 1.79(6) . . . . ?
O5 W2 N1 P 107.84(8) . . . . ?
O4 W2 N1 P -118.34(7) . . . . ?
W1 W2 N1 P -1.94(7) . . . . ?
O5 W2 N1 Si1 -60.64(11) . . . . ?
O4 W2 N1 Si1 73.18(11) . . . . ?
W1 W2 N1 Si1 -170.43(9) . . . . ?
P W2 N1 Si1 -168.48(15) . . . . ?
P N1 Si1 C2 -1.03(18) . . . . ?
W2 N1 Si1 C2 161.95(11) . . . . ?
P N1 Si1 C3 -123.15(15) . . . . ?
W2 N1 Si1 C3 39.83(13) . . . . ?
P N1 Si1 C1 120.75(15) . . . . ?
W2 N1 Si1 C1 -76.27(13) . . . . ?
O6 P N2 Si2 -154.40(11) . . . . ?
N1 P N2 Si2 -46.18(13) . . . . ?
W1 P N2 Si2 68.20(12) . . . . ?
W2 P N2 Si2 0.83(15) . . . . ?
O6 P N2 Si3 27.84(10) . . . . ?
N1 P N2 Si3 136.07(10) . . . . ?
W1 P N2 Si3 -109.55(9) . . . . ?
W2 P N2 Si3 -176.93(4) . . . . ?
O2 W1 O1 C11 -42.60(14) . . . . ?
O3 W1 O1 C11 51.92(18) . . . . ?
W2 W1 O1 C11 -158.47(12) . . . . ?
P W1 O1 C11 134.33(13) . . . . ?
W1 O1 C11 C12 152.47(13) . . . . ?
W1 O1 C11 C10 -84.09(17) . . . . ?
O1 W1 O2 C14 -101.05(17) . . . . ?
O3 W1 O2 C14 110.74(17) . . . . ?
W2 W1 O2 C14 5.14(18) . . . . ?
W1 O2 C14 C15 -127.32(17) . . . . ?
W1 O2 C14 C13 110.71(18) . . . . ?
O1 W1 O3 C17 -53.62(19) . . . . ?
O2 W1 O3 C17 41.25(15) . . . . ?
W2 W1 O3 C17 156.78(13) . . . . ?
P W1 O3 C17 -135.50(14) . . . . ?
W1 O3 C17 C18 -143.1(2) . . . . ?
W1 O3 C17 C16 93.4(2) . . . . ?
O5 W2 O4 C20 -102.80(19) . . . . ?
N1 W2 O4 C20 120.27(19) . . . . ?
W1 W2 O4 C20 12.0(2) . . . . ?
P W2 O4 C20 78.3(2) . . . . ?
W2 O4 C20 C19 -136.69(17) . . . . ?
W2 O4 C20 C21 102.1(2) . . . . ?
O4 W2 O5 C23 97.78(18) . . . . ?
N1 W2 O5 C23 -125.19(17) . . . . ?
W1 W2 O5 C23 -20.53(18) . . . . ?
P W2 O5 C23 -83.23(18) . . . . ?
W2 O5 C23 C22 128.73(17) . . . . ?
W2 O5 C23 C24 -108.83(19) . . . . ?
P N2 Si2 C4 -3.78(15) . . . . ?
Si3 N2 Si2 C4 173.93(10) . . . . ?
P N2 Si2 C6 117.00(13) . . . . ?
Si3 N2 Si2 C6 -65.30(13) . . . . ?
P N2 Si2 C5 -122.24(12) . . . . ?
Si3 N2 Si2 C5 55.47(13) . . . . ?
P N2 Si3 C7 48.29(13) . . . . ?
Si2 N2 Si3 C7 -129.58(11) . . . . ?
P N2 Si3 C9 -80.33(13) . . . . ?
Si2 N2 Si3 C9 101.81(13) . . . . ?
P N2 Si3 C8 163.50(11) . . . . ?
Si2 N2 Si3 C8 -14.37(14) . . . . ?
N1 P O6 C26 88.57(16) . . . . ?
N2 P O6 C26 -158.93(16) . . . . ?
W1 P O6 C26 -21.31(17) . . . . ?
W2 P O6 C26 43.06(17) . . . . ?
P O6 C26 C25 -75.9(2) . . . . ?
P O6 C26 C27 162.96(14) . . . . ?
