#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:22:22 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178561 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/69/4066906.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_4066906
loop_
_publ_author_name
'Semenov, Sergey N.'
'Blacque, Olivier'
'Fox, Thomas'
'Venkatesan, Koushik'
'Berke, Heinz'
_publ_section_title
;
 [W(CO)(dppe)2] Cumulenylidene and Acetylide Complexes Accessed via
 Stannylated Acetylenes and Butadiynes
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6321
_journal_paper_doi               10.1021/om100702x
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C61 H66 O P4 Sn2 W, 0.5(C6 H6)'
_chemical_formula_sum            'C64 H69 O P4 Sn2 W'
_chemical_formula_weight         1399.34
_chemical_name_systematic
'[cis-(2,2'-ditrimethylstannylvinylidene)bis{1,2-bis(diphenylphosphino)ethane}carbonyltungsten]'
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.344(2)
_cell_angle_beta                 102.127(2)
_cell_angle_gamma                99.800(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0392(3)
_cell_length_b                   12.1400(3)
_cell_length_c                   21.6189(5)
_cell_measurement_reflns_used    17320
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.76
_cell_measurement_theta_min      2.24
_cell_volume                     2940.25(13)
_computing_cell_refinement
' CrysAlisPro Software, Oxford Diffraction Ltd., Version 1.171.32.24'
_computing_data_collection
' CrysAlisPro Software, Oxford Diffraction Ltd., Version 1.171.32.24'
_computing_data_reduction
' CrysAlisPro Software, Oxford Diffraction Ltd., Version 1.171.32.24'
_computing_molecular_graphics
; ORTEP-3 for Windows, Version 2.01.
  Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
;
_computing_publication_material
; WinGX -- An integrated system of Windows programs for the solution,
 refinment and analysis of single crystal X-ray diffraction data,
 Version 1.80.00.
 Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
 SHELXL97. Program for crystal structure refinement.
 Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
 PLATON for Windows, Version 1.12.
 Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. 
;
_computing_structure_refinement
; SHELXL97. Program for crystal structure refinement.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_solution
; SHELXS97. Program for Crystal Structure solution.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.  
;
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
; Oxford Diffraction (2007). Oxford Diffraction Ltd., 
Xcalibur CCD system
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0937
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            44093
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  105
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    2.943
_exptl_absorpt_correction_T_max  0.833
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
R.C. Clark and J.S. Reid, Acta Cryst. 1995, A51, 887-897
implemented in the CrysAlis Software system, Oxford Diffraction Ltd.,
Version 1.171.32.24
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1390
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.572
_refine_diff_density_min         -1.930
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         17891
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0490P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1100
_reflns_number_gt                12592
_reflns_number_total             17891
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100702x_si_002.cif
_cod_data_source_block           6
_cod_original_cell_volume        2940.26(13)
_cod_database_code               4066906
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
C1 C 0.9294(4) 0.0413(4) 0.6791(2) 0.0233(9) Uani 1 1 d .
C2 C 0.9166(4) -0.0534(4) 0.8982(2) 0.0301(11) Uani 1 1 d .
H2A H 0.8949 -0.0933 0.9297 0.036 Uiso 1 1 calc R
H2B H 0.9849 0.0082 0.9207 0.036 Uiso 1 1 calc R
C3 C 0.8158(4) -0.0019(4) 0.8692(2) 0.0289(10) Uani 1 1 d .
H3A H 0.8009 0.0552 0.9035 0.035 Uiso 1 1 calc R
H3B H 0.7454 -0.0625 0.8499 0.035 Uiso 1 1 calc R
C4 C 1.0851(4) -0.1881(4) 0.8771(2) 0.0269(10) Uani 1 1 d .
C5 C 1.1231(5) -0.2809(5) 0.8458(3) 0.0360(12) Uani 1 1 d .
H5 H 1.0803 -0.3246 0.8042 0.043 Uiso 1 1 calc R
C6 C 1.2239(5) -0.3099(5) 0.8756(3) 0.0418(13) Uani 1 1 d .
H6 H 1.2482 -0.3727 0.8541 0.050 Uiso 1 1 calc R
C7 C 1.2878(5) -0.2450(5) 0.9372(3) 0.0456(15) Uani 1 1 d .
H7 H 1.3563 -0.2630 0.9572 0.055 Uiso 1 1 calc R
C8 C 1.2499(5) -0.1537(6) 0.9691(3) 0.0432(14) Uani 1 1 d .
H8 H 1.2922 -0.1106 1.0110 0.052 Uiso 1 1 calc R
C9 C 1.1485(4) -0.1253(5) 0.9390(2) 0.0344(12) Uani 1 1 d .
H9 H 1.1234 -0.0633 0.9609 0.041 Uiso 1 1 calc R
C10 C 0.8446(4) -0.2884(4) 0.8258(2) 0.0288(10) Uani 1 1 d .
C11 C 0.8692(6) -0.3710(6) 0.8597(3) 0.065(2) Uani 1 1 d .
H11 H 0.9427 -0.3597 0.8876 0.078 Uiso 1 1 calc R
C12 C 0.7846(7) -0.4698(7) 0.8517(4) 0.086(3) Uani 1 1 d .
H12 H 0.8021 -0.5245 0.8743 0.103 Uiso 1 1 calc R
C13 C 0.6762(6) -0.4875(6) 0.8112(4) 0.064(2) Uani 1 1 d .
H13 H 0.6196 -0.5535 0.8064 0.076 Uiso 1 1 calc R
C14 C 0.6519(5) -0.4084(6) 0.7783(3) 0.0518(16) Uani 1 1 d .
H14 H 0.5778 -0.4195 0.7510 0.062 Uiso 1 1 calc R
C15 C 0.7361(5) -0.3106(5) 0.7845(3) 0.0377(13) Uani 1 1 d .
H15 H 0.7182 -0.2588 0.7599 0.045 Uiso 1 1 calc R
C16 C 0.9402(4) 0.2128(4) 0.8545(2) 0.0248(10) Uani 1 1 d .
C17 C 0.9858(4) 0.2848(4) 0.8198(2) 0.0291(11) Uani 1 1 d .
H17 H 0.9736 0.2577 0.7747 0.035 Uiso 1 1 calc R
C18 C 1.0488(5) 0.3958(5) 0.8509(3) 0.0402(13) Uani 1 1 d .
H18 H 1.0777 0.4429 0.8265 0.048 Uiso 1 1 calc R
C19 C 1.0697(5) 0.4382(5) 0.9179(3) 0.0429(14) Uani 1 1 d .
H19 H 1.1132 0.5129 0.9390 0.051 Uiso 1 1 calc R
C20 C 1.0242(5) 0.3668(5) 0.9527(2) 0.0406(13) Uani 1 1 d .
H20 H 1.0371 0.3940 0.9977 0.049 Uiso 1 1 calc R
C21 C 0.9595(5) 0.2550(5) 0.9215(2) 0.0351(12) Uani 1 1 d .
H21 H 0.9292 0.2084 0.9457 0.042 Uiso 1 1 calc R
C22 C 0.7218(4) 0.1110(4) 0.7726(2) 0.0288(10) Uani 1 1 d .
C23 C 0.6869(4) 0.1059(5) 0.7072(3) 0.0378(13) Uani 1 1 d .
H23 H 0.7280 0.0750 0.6785 0.045 Uiso 1 1 calc R
C24 C 0.5888(5) 0.1474(5) 0.6841(3) 0.0510(16) Uani 1 1 d .
H24 H 0.5670 0.1467 0.6401 0.061 Uiso 1 1 calc R
C25 C 0.5241(5) 0.1893(5) 0.7254(4) 0.0525(17) Uani 1 1 d .
H25 H 0.4572 0.2137 0.7092 0.063 Uiso 1 1 calc R
C26 C 0.5594(5) 0.1945(5) 0.7900(4) 0.0545(17) Uani 1 1 d .
H26 H 0.5171 0.2241 0.8184 0.065 Uiso 1 1 calc R
C27 C 0.6574(5) 0.1564(5) 0.8143(3) 0.0434(14) Uani 1 1 d .
H27 H 0.6806 0.1611 0.8588 0.052 Uiso 1 1 calc R
C28 C 1.2342(4) -0.0537(4) 0.7241(2) 0.0279(10) Uani 1 1 d .
H28A H 1.2250 -0.0403 0.6809 0.033 Uiso 1 1 calc R
H28B H 1.3168 -0.0326 0.7460 0.033 Uiso 1 1 calc R
C29 C 1.1870(4) -0.1812(4) 0.7177(2) 0.0280(10) Uani 1 1 d .
H29A H 1.2015 -0.1970 0.7604 0.034 Uiso 1 1 calc R
H29B H 1.2245 -0.2288 0.6904 0.034 Uiso 1 1 calc R
C30 C 1.2457(4) 0.0725(4) 0.8567(2) 0.0285(11) Uani 1 1 d .
C31 C 1.3495(5) 0.0384(5) 0.8757(3) 0.0393(13) Uani 1 1 d .
H31 H 1.3768 -0.0072 0.8445 0.047 Uiso 1 1 calc R
C32 C 1.4124(5) 0.0716(6) 0.9405(3) 0.0487(16) Uani 1 1 d .
H32 H 1.4818 0.0483 0.9523 0.058 Uiso 1 1 calc R
C33 C 1.3741(6) 0.1387(6) 0.9879(3) 0.0544(18) Uani 1 1 d .
H33 H 1.4168 0.1599 1.0315 0.065 Uiso 1 1 calc R
C34 C 1.2725(6) 0.1738(5) 0.9704(3) 0.0483(15) Uani 1 1 d .
H34 H 1.2467 0.2203 1.0019 0.058 Uiso 1 1 calc R
C35 C 1.2084(5) 0.1403(5) 0.9059(2) 0.0352(12) Uani 1 1 d .
H35 H 1.1386 0.1634 0.8948 0.042 Uiso 1 1 calc R
C36 C 1.2085(4) 0.1738(4) 0.7493(2) 0.0261(10) Uani 1 1 d .
C37 C 1.1877(4) 0.1738(5) 0.6848(3) 0.0372(12) Uani 1 1 d .
H37 H 1.1446 0.1069 0.6532 0.045 Uiso 1 1 calc R
C38 C 1.2292(5) 0.2713(6) 0.6648(3) 0.0468(15) Uani 1 1 d .
H38 H 1.2148 0.2684 0.6204 0.056 Uiso 1 1 calc R
C39 C 1.2907(5) 0.3704(5) 0.7099(4) 0.0518(17) Uani 1 1 d .
H39 H 1.3188 0.4354 0.6967 0.062 Uiso 1 1 calc R
C40 C 1.3110(5) 0.3742(5) 0.7750(4) 0.0499(16) Uani 1 1 d .
H40 H 1.3524 0.4422 0.8061 0.060 Uiso 1 1 calc R
C41 C 1.2703(4) 0.2771(4) 0.7951(3) 0.0358(12) Uani 1 1 d .
H41 H 1.2843 0.2810 0.8396 0.043 Uiso 1 1 calc R
C42 C 1.0387(4) -0.2268(4) 0.5951(2) 0.0257(10) Uani 1 1 d .
C43 C 1.0754(5) -0.3203(5) 0.5618(3) 0.0357(12) Uani 1 1 d .
H43 H 1.0902 -0.3789 0.5817 0.043 Uiso 1 1 calc R
C44 C 1.0899(5) -0.3264(5) 0.4992(2) 0.0397(13) Uani 1 1 d .
H44 H 1.1151 -0.3885 0.4776 0.048 Uiso 1 1 calc R
C45 C 1.0670(6) -0.2409(5) 0.4689(3) 0.0461(15) Uani 1 1 d .
H45 H 1.0782 -0.2445 0.4273 0.055 Uiso 1 1 calc R
C46 C 1.0276(5) -0.1501(5) 0.5003(2) 0.0418(14) Uani 1 1 d .
H46 H 1.0103 -0.0936 0.4792 0.050 Uiso 1 1 calc R
C47 C 1.0134(5) -0.1418(4) 0.5633(2) 0.0337(12) Uani 1 1 d .
H47 H 0.9872 -0.0799 0.5841 0.040 Uiso 1 1 calc R
C48 C 0.9766(4) -0.3655(4) 0.6786(2) 0.0259(10) Uani 1 1 d .
C49 C 0.8576(4) -0.4061(4) 0.6667(2) 0.0320(11) Uani 1 1 d .
H49 H 0.8078 -0.3568 0.6595 0.038 Uiso 1 1 calc R
C50 C 0.8116(5) -0.5199(5) 0.6653(3) 0.0398(13) Uani 1 1 d .
H50 H 0.7314 -0.5465 0.6572 0.048 Uiso 1 1 calc R
C51 C 0.8856(5) -0.5941(4) 0.6761(2) 0.0368(12) Uani 1 1 d .
H51 H 0.8555 -0.6699 0.6761 0.044 Uiso 1 1 calc R
C52 C 1.0025(5) -0.5545(4) 0.6867(2) 0.0347(12) Uani 1 1 d .
H52 H 1.0519 -0.6042 0.6936 0.042 Uiso 1 1 calc R
C53 C 1.0492(4) -0.4423(4) 0.6875(2) 0.0317(11) Uani 1 1 d .
H53 H 1.1292 -0.4176 0.6939 0.038 Uiso 1 1 calc R
C54 C 0.7806(4) -0.1446(4) 0.6812(2) 0.0237(9) Uani 1 1 d .
C55 C 0.6801(4) -0.1905(4) 0.6395(2) 0.0280(10) Uani 1 1 d .
C56 C 0.4075(5) -0.1156(6) 0.6056(3) 0.0477(15) Uani 1 1 d .
H56A H 0.3346 -0.1678 0.5813 0.072 Uiso 1 1 calc R
H56B H 0.4475 -0.0884 0.5758 0.072 Uiso 1 1 calc R
H56C H 0.3931 -0.0510 0.6347 0.072 Uiso 1 1 calc R
C57 C 0.4239(6) -0.3824(5) 0.6308(3) 0.0575(18) Uani 1 1 d .
H57A H 0.3566 -0.3938 0.5952 0.086 Uiso 1 1 calc R
H57B H 0.3999 -0.4047 0.6668 0.086 Uiso 1 1 calc R
H57C H 0.4755 -0.4289 0.6167 0.086 Uiso 1 1 calc R
C58 C 0.5122(5) -0.1522(5) 0.7628(3) 0.0438(14) Uani 1 1 d .
H58A H 0.5323 -0.0692 0.7779 0.066 Uiso 1 1 calc R
H58B H 0.5682 -0.1835 0.7883 0.066 Uiso 1 1 calc R
H58C H 0.4360 -0.1808 0.7677 0.066 Uiso 1 1 calc R
C59 C 0.7180(6) -0.0856(6) 0.5049(3) 0.0605(19) Uani 1 1 d .
H59A H 0.6569 -0.0440 0.5024 0.091 Uiso 1 1 calc R
H59B H 0.7329 -0.1073 0.4626 0.091 Uiso 1 1 calc R
H59C H 0.7876 -0.0373 0.5358 0.091 Uiso 1 1 calc R
C60 C 0.7557(5) -0.3692(5) 0.5072(3) 0.0498(15) Uani 1 1 d .
H60A H 0.8382 -0.3372 0.5209 0.075 Uiso 1 1 calc R
H60B H 0.7320 -0.3986 0.4604 0.075 Uiso 1 1 calc R
H60C H 0.7372 -0.4311 0.5272 0.075 Uiso 1 1 calc R
C61 C 0.4875(6) -0.3154(7) 0.4802(3) 0.070(2) Uani 1 1 d .
H61A H 0.4607 -0.3858 0.4915 0.105 Uiso 1 1 calc R
H61B H 0.4838 -0.3321 0.4343 0.105 Uiso 1 1 calc R
H61C H 0.4388 -0.2626 0.4901 0.105 Uiso 1 1 calc R
O1 O 0.9206(3) 0.1080(3) 0.64659(16) 0.0340(8) Uani 1 1 d .
P1 P 0.95067(11) -0.15529(11) 0.83253(6) 0.0237(2) Uani 1 1 d .
P2 P 0.85611(11) 0.06647(10) 0.80616(6) 0.0238(2) Uani 1 1 d .
P3 P 1.15658(10) 0.03802(11) 0.77145(6) 0.0230(2) Uani 1 1 d .
P4 P 1.02861(10) -0.21269(10) 0.67987(6) 0.0224(2) Uani 1 1 d .
Sn1 Sn 0.51261(3) -0.20364(3) 0.661212(17) 0.03275(9) Uani 1 1 d .
Sn2 Sn 0.66593(3) -0.23787(3) 0.536160(17) 0.03724(10) Uani 1 1 d .
W1 W 0.941210(15) -0.061844(16) 0.736296(8) 0.01847(5) Uani 1 1 d .
C62 C 1.406(2) -0.479(3) 1.0293(15) 0.478(15) Uani 1 1 d D
H62 H 1.3458 -0.4646 1.0481 0.574 Uiso 1 1 calc R
C63 C 1.3861(10) -0.530(3) 0.9621(13) 0.478(15) Uani 1 1 d D
H63 H 1.3099 -0.5525 0.9361 0.574 Uiso 1 1 calc R
C64 C 1.478(3) -0.5488(18) 0.9331(3) 0.478(15) Uani 1 1 d D
H64 H 1.4610 -0.5802 0.8881 0.574 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'
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'
Sn Sn -0.6537 1.4246 '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
O1 C1 W1 176.6(4) .
C3 C2 P1 110.0(3) .
C3 C2 H2A 109.7 .
P1 C2 H2A 109.7 .
C3 C2 H2B 109.7 .
P1 C2 H2B 109.7 .
H2A C2 H2B 108.2 .
C2 C3 P2 108.7(3) .
C2 C3 H3A 109.9 .
P2 C3 H3A 109.9 .
C2 C3 H3B 109.9 .
P2 C3 H3B 109.9 .
H3A C3 H3B 108.3 .
C9 C4 C5 118.8(4) .
C9 C4 P1 123.6(4) .
C5 C4 P1 117.6(3) .
C4 C5 C6 121.1(5) .
C4 C5 H5 119.5 .
C6 C5 H5 119.5 .
C7 C6 C5 119.6(5) .
C7 C6 H6 120.2 .
C5 C6 H6 120.2 .
C8 C7 C6 119.7(5) .
C8 C7 H7 120.1 .
C6 C7 H7 120.1 .
C7 C8 C9 120.3(5) .
C7 C8 H8 119.9 .
C9 C8 H8 119.9 .
C4 C9 C8 120.5(5) .
C4 C9 H9 119.8 .
C8 C9 H9 119.8 .
C15 C10 C11 117.2(5) .
C15 C10 P1 119.1(4) .
C11 C10 P1 123.7(4) .
C12 C11 C10 120.3(6) .
C12 C11 H11 119.8 .
C10 C11 H11 119.8 .
C13 C12 C11 120.7(7) .
C13 C12 H12 119.7 .
C11 C12 H12 119.7 .
C14 C13 C12 119.3(6) .
C14 C13 H13 120.3 .
C12 C13 H13 120.3 .
C13 C14 C15 120.7(6) .
C13 C14 H14 119.6 .
C15 C14 H14 119.6 .
C10 C15 C14 121.7(5) .
C10 C15 H15 119.2 .
C14 C15 H15 119.2 .
C17 C16 C21 118.5(5) .
C17 C16 P2 116.4(3) .
C21 C16 P2 125.2(4) .
C18 C17 C16 121.1(5) .
C18 C17 H17 119.5 .
C16 C17 H17 119.5 .
C17 C18 C19 120.9(5) .
C17 C18 H18 119.6 .
C19 C18 H18 119.6 .
C20 C19 C18 118.2(5) .
C20 C19 H19 120.9 .
C18 C19 H19 120.9 .
C19 C20 C21 121.2(5) .
C19 C20 H20 119.4 .
C21 C20 H20 119.4 .
C16 C21 C20 120.1(5) .
C16 C21 H21 119.9 .
C20 C21 H21 119.9 .
C23 C22 C27 118.8(5) .
C23 C22 P2 121.0(4) .
C27 C22 P2 120.1(4) .
C22 C23 C24 119.5(5) .
C22 C23 H23 120.3 .
C24 C23 H23 120.3 .
C25 C24 C23 121.2(6) .
C25 C24 H24 119.4 .
C23 C24 H24 119.4 .
C26 C25 C24 118.9(5) .
C26 C25 H25 120.5 .
C24 C25 H25 120.5 .
C25 C26 C27 120.9(6) .
C25 C26 H26 119.5 .
C27 C26 H26 119.5 .
C26 C27 C22 120.6(6) .
C26 C27 H27 119.7 .
C22 C27 H27 119.7 .
C29 C28 P3 110.9(3) .
C29 C28 H28A 109.5 .
P3 C28 H28A 109.5 .
C29 C28 H28B 109.5 .
P3 C28 H28B 109.5 .
H28A C28 H28B 108.0 .
C28 C29 P4 106.9(3) .
C28 C29 H29A 110.3 .
P4 C29 H29A 110.3 .
C28 C29 H29B 110.3 .
P4 C29 H29B 110.3 .
H29A C29 H29B 108.6 .
C31 C30 C35 117.2(4) .
C31 C30 P3 124.7(4) .
C35 C30 P3 118.1(4) .
C32 C31 C30 120.6(5) .
C32 C31 H31 119.7 .
C30 C31 H31 119.7 .
C33 C32 C31 121.1(5) .
C33 C32 H32 119.5 .
C31 C32 H32 119.5 .
C34 C33 C32 119.4(5) .
C34 C33 H33 120.3 .
C32 C33 H33 120.3 .
C33 C34 C35 120.0(6) .
C33 C34 H34 120.0 .
C35 C34 H34 120.0 .
C34 C35 C30 121.7(5) .
C34 C35 H35 119.2 .
C30 C35 H35 119.2 .
C37 C36 C41 117.1(5) .
C37 C36 P3 119.1(4) .
C41 C36 P3 123.8(4) .
C36 C37 C38 121.9(6) .
C36 C37 H37 119.1 .
C38 C37 H37 119.1 .
C39 C38 C37 120.2(6) .
C39 C38 H38 119.9 .
C37 C38 H38 119.9 .
C38 C39 C40 119.5(6) .
C38 C39 H39 120.2 .
C40 C39 H39 120.2 .
C39 C40 C41 120.6(6) .
C39 C40 H40 119.7 .
C41 C40 H40 119.7 .
C40 C41 C36 120.7(5) .
C40 C41 H41 119.6 .
C36 C41 H41 119.6 .
C47 C42 C43 118.5(4) .
C47 C42 P4 120.4(4) .
C43 C42 P4 121.0(4) .
C44 C43 C42 120.6(5) .
C44 C43 H43 119.7 .
C42 C43 H43 119.7 .
C45 C44 C43 120.3(5) .
C45 C44 H44 119.9 .
C43 C44 H44 119.9 .
C44 C45 C46 119.9(5) .
C44 C45 H45 120.1 .
C46 C45 H45 120.1 .
C45 C46 C47 120.7(5) .
C45 C46 H46 119.6 .
C47 C46 H46 119.6 .
C46 C47 C42 119.9(5) .
C46 C47 H47 120.0 .
C42 C47 H47 120.0 .
C49 C48 C53 118.5(5) .
C49 C48 P4 117.2(4) .
C53 C48 P4 124.3(4) .
C48 C49 C50 120.7(5) .
C48 C49 H49 119.7 .
C50 C49 H49 119.7 .
C49 C50 C51 119.9(5) .
C49 C50 H50 120.0 .
C51 C50 H50 120.0 .
C52 C51 C50 119.3(5) .
C52 C51 H51 120.4 .
C50 C51 H51 120.4 .
C51 C52 C53 121.4(5) .
C51 C52 H52 119.3 .
C53 C52 H52 119.3 .
C52 C53 C48 120.2(5) .
C52 C53 H53 119.9 .
C48 C53 H53 119.9 .
C55 C54 W1 171.9(4) .
C54 C55 Sn2 120.9(4) .
C54 C55 Sn1 126.0(4) .
Sn2 C55 Sn1 112.4(2) .
Sn1 C56 H56A 109.5 .
Sn1 C56 H56B 109.5 .
H56A C56 H56B 109.5 .
Sn1 C56 H56C 109.5 .
H56A C56 H56C 109.5 .
H56B C56 H56C 109.5 .
Sn1 C57 H57A 109.5 .
Sn1 C57 H57B 109.5 .
H57A C57 H57B 109.5 .
Sn1 C57 H57C 109.5 .
H57A C57 H57C 109.5 .
H57B C57 H57C 109.5 .
Sn1 C58 H58A 109.5 .
Sn1 C58 H58B 109.5 .
H58A C58 H58B 109.5 .
Sn1 C58 H58C 109.5 .
H58A C58 H58C 109.5 .
H58B C58 H58C 109.5 .
Sn2 C59 H59A 109.5 .
Sn2 C59 H59B 109.5 .
H59A C59 H59B 109.5 .
Sn2 C59 H59C 109.5 .
H59A C59 H59C 109.5 .
H59B C59 H59C 109.5 .
Sn2 C60 H60A 109.5 .
Sn2 C60 H60B 109.5 .
H60A C60 H60B 109.5 .
Sn2 C60 H60C 109.5 .
H60A C60 H60C 109.5 .
H60B C60 H60C 109.5 .
Sn2 C61 H61A 109.5 .
Sn2 C61 H61B 109.5 .
H61A C61 H61B 109.5 .
Sn2 C61 H61C 109.5 .
H61A C61 H61C 109.5 .
H61B C61 H61C 109.5 .
C2 P1 C10 100.7(2) .
C2 P1 C4 101.7(2) .
C10 P1 C4 99.8(2) .
C2 P1 W1 106.49(16) .
C10 P1 W1 120.79(15) .
C4 P1 W1 123.75(16) .
C22 P2 C3 102.5(2) .
C22 P2 C16 96.3(2) .
C3 P2 C16 103.0(2) .
C22 P2 W1 121.47(17) .
C3 P2 W1 109.59(16) .
C16 P2 W1 121.12(15) .
C30 P3 C28 103.8(2) .
C30 P3 C36 100.2(2) .
C28 P3 C36 97.2(2) .
C30 P3 W1 123.03(17) .
C28 P3 W1 107.91(16) .
C36 P3 W1 120.76(14) .
C42 P4 C48 101.1(2) .
C42 P4 C29 96.6(2) .
C48 P4 C29 104.2(2) .
C42 P4 W1 122.01(16) .
C48 P4 W1 119.48(16) .
C29 P4 W1 109.87(15) .
C56 Sn1 C57 106.6(2) .
C56 Sn1 C55 110.6(2) .
C57 Sn1 C55 108.2(2) .
C56 Sn1 C58 110.2(2) .
C57 Sn1 C58 103.6(3) .
C55 Sn1 C58 116.93(19) .
C60 Sn2 C59 112.7(3) .
C60 Sn2 C55 113.7(2) .
C59 Sn2 C55 109.3(2) .
C60 Sn2 C61 102.8(3) .
C59 Sn2 C61 106.2(3) .
C55 Sn2 C61 111.7(2) .
C1 W1 C54 84.19(19) .
C1 W1 P2 86.72(13) .
C54 W1 P2 89.61(13) .
C1 W1 P4 103.46(13) .
C54 W1 P4 91.45(13) .
P2 W1 P4 169.82(4) .
C1 W1 P3 84.21(14) .
C54 W1 P3 162.29(13) .
P2 W1 P3 103.03(4) .
P4 W1 P3 78.32(4) .
C1 W1 P1 165.79(13) .
C54 W1 P1 99.85(13) .
P2 W1 P1 79.73(4) .
P4 W1 P1 90.12(4) .
P3 W1 P1 94.64(4) .
C64 C62 C63 116.9(5) 2_847
C64 C62 H62 121.6 2_847
C63 C62 H62 121.6 .
C62 C63 C64 122.0(19) .
C62 C63 H63 119.1 .
C64 C63 H63 119.1 .
C62 C64 C63 121.3(5) 2_847
C62 C64 H64 119.4 2_847
C63 C64 H64 119.4 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.184(5) .
C1 W1 1.940(5) .
C2 C3 1.536(6) .
C2 P1 1.838(5) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 P2 1.847(5) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 C9 1.374(7) .
C4 C5 1.385(7) .
C4 P1 1.853(5) .
C5 C6 1.387(7) .
C5 H5 0.9300 .
C6 C7 1.380(8) .
C6 H6 0.9300 .
C7 C8 1.375(8) .
C7 H7 0.9300 .
C8 C9 1.393(7) .
C8 H8 0.9300 .
C9 H9 0.9300 .
C10 C15 1.365(7) .
C10 C11 1.397(7) .
C10 P1 1.839(5) .
C11 C12 1.389(9) .
C11 H11 0.9300 .
C12 C13 1.364(9) .
C12 H12 0.9300 .
C13 C14 1.348(8) .
C13 H13 0.9300 .
C14 C15 1.385(8) .
C14 H14 0.9300 .
C15 H15 0.9300 .
C16 C17 1.384(7) .
C16 C21 1.385(6) .
C16 P2 1.850(5) .
C17 C18 1.376(7) .
C17 H17 0.9300 .
C18 C19 1.384(7) .
C18 H18 0.9300 .
C19 C20 1.380(8) .
C19 H19 0.9300 .
C20 C21 1.390(8) .
C20 H20 0.9300 .
C21 H21 0.9300 .
C22 C23 1.372(7) .
C22 C27 1.394(7) .
C22 P2 1.845(5) .
C23 C24 1.400(7) .
C23 H23 0.9300 .
C24 C25 1.376(9) .
C24 H24 0.9300 .
C25 C26 1.358(9) .
C25 H25 0.9300 .
C26 C27 1.382(8) .
C26 H26 0.9300 .
C27 H27 0.9300 .
C28 C29 1.521(7) .
C28 P3 1.852(5) .
C28 H28A 0.9700 .
C28 H28B 0.9700 .
C29 P4 1.848(5) .
C29 H29A 0.9700 .
C29 H29B 0.9700 .
C30 C31 1.392(7) .
C30 C35 1.401(7) .
C30 P3 1.847(5) .
C31 C32 1.380(7) .
C31 H31 0.9300 .
C32 C33 1.377(9) .
C32 H32 0.9300 .
C33 C34 1.368(9) .
C33 H33 0.9300 .
C34 C35 1.380(7) .
C34 H34 0.9300 .
C35 H35 0.9300 .
C36 C37 1.366(7) .
C36 C41 1.396(7) .
C36 P3 1.857(5) .
C37 C38 1.395(8) .
C37 H37 0.9300 .
C38 C39 1.356(9) .
C38 H38 0.9300 .
C39 C40 1.365(9) .
C39 H39 0.9300 .
C40 C41 1.390(8) .
C40 H40 0.9300 .
C41 H41 0.9300 .
C42 C47 1.398(7) .
C42 C43 1.399(6) .
C42 P4 1.834(5) .
C43 C44 1.388(7) .
C43 H43 0.9300 .
C44 C45 1.376(8) .
C44 H44 0.9300 .
C45 C46 1.377(8) .
C45 H45 0.9300 .
C46 C47 1.393(7) .
C46 H46 0.9300 .
C47 H47 0.9300 .
C48 C49 1.383(7) .
C48 C53 1.397(6) .
C48 P4 1.847(5) .
C49 C50 1.390(7) .
C49 H49 0.9300 .
C50 C51 1.391(7) .
C50 H50 0.9300 .
C51 C52 1.360(8) .
C51 H51 0.9300 .
C52 C53 1.378(7) .
C52 H52 0.9300 .
C53 H53 0.9300 .
C54 C55 1.298(6) .
C54 W1 2.007(4) .
C55 Sn2 2.146(5) .
C55 Sn1 2.153(5) .
C56 Sn1 2.135(5) .
C56 H56A 0.9600 .
C56 H56B 0.9600 .
C56 H56C 0.9600 .
C57 Sn1 2.142(6) .
C57 H57A 0.9600 .
C57 H57B 0.9600 .
C57 H57C 0.9600 .
C58 Sn1 2.153(5) .
C58 H58A 0.9600 .
C58 H58B 0.9600 .
C58 H58C 0.9600 .
C59 Sn2 2.141(7) .
C59 H59A 0.9600 .
C59 H59B 0.9600 .
C59 H59C 0.9600 .
C60 Sn2 2.133(6) .
C60 H60A 0.9600 .
C60 H60B 0.9600 .
C60 H60C 0.9600 .
C61 Sn2 2.167(6) .
C61 H61A 0.9600 .
C61 H61B 0.9600 .
C61 H61C 0.9600 .
P1 W1 2.5655(12) .
P2 W1 2.4383(12) .
P3 W1 2.5453(12) .
P4 W1 2.4878(12) .
C62 C64 1.40(4) 2_847
C62 C63 1.40(4) .
C62 H62 0.9300 .
C63 C64 1.41(4) .
C63 H63 0.9300 .
C64 C62 1.40(4) 2_847
C64 H64 0.9300 .
