[W(CO)(dppe)2] Cumulenylidene and Acetylide Complexes Accessed via Stannylated Acetylenes and Butadiynes
Semenov, Sergey N.; Blacque, Olivier; Fox, Thomas; Venkatesan, Koushik; Berke, Heinz; Organometallics 29 (2010) 6321–; doi:10.1021/om100702x

data_4066909
_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         'C57 H49 O P4 W, C16 H36 N'
_chemical_formula_sum            'C73 H85 N O P4 W'
_chemical_formula_weight         1300.14
_chemical_name_systematic
;
[Trans-(butadiynyl)bis{1,2-bis(diphenylphosphino)ethane}carbonyltungstate]
tetrabuthylammonium
;
_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                77.567(4)
_cell_angle_beta                 88.606(5)
_cell_angle_gamma                89.185(4)
_cell_formula_units_Z            4
_cell_length_a                   12.2029(9)
_cell_length_b                   21.5463(9)
_cell_length_c                   25.0892(12)
_cell_measurement_reflns_used    5306
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.85
_cell_measurement_theta_min      2.47
_cell_volume                     6439.8(6)
_computing_cell_refinement
;
CrysAlisPro Software, Oxford Diffraction Ltd.,
Version 1.171.33.55 
;
_computing_data_collection
;
CrysAlisPro Software, Oxford Diffraction Ltd.,
Version 1.171.33.55
;
_computing_data_reduction
;
CrysAlisPro Software, Oxford Diffraction Ltd.,
Version 1.171.33.55 
;
_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      153(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
; Goniometer Xcalibur, detector: Ruby
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  0.1113
_diffrn_reflns_av_sigmaI/netI    0.5079
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            45824
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.937
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tiny plate'
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.619
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1448
_refine_ls_number_reflns         22679
_refine_ls_number_restraints     511
_refine_ls_restrained_S_all      0.637
_refine_ls_R_factor_all          0.2276
_refine_ls_R_factor_gt           0.0531
_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/[\s^2^(Fo^2^)+(0.0000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0747
_reflns_number_gt                6076
_reflns_number_total             22679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100702x_si_002.cif
_cod_data_source_block           10
_cod_database_code               4066909