Electronic Communication in Dinuclear C4-Bridged Tungsten Complexes
Sergey N. Semenov; Olivier Blacque; Thomas Fox; Koushik Venkatesan; Heinz Berke; Journal of the American Chemical Society 132 (2010) 3115–3127; doi:10.1021/ja909764x

data_4102012
_publ_section_title
;
 Electronic Communication in Dinuclear C4-Bridged Tungsten Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3115
_journal_page_last               3127
_journal_paper_doi               10.1021/ja909764x
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C37 H29 I O3 P2 W'
_chemical_formula_sum            'C37 H29 I O3 P2 W'
_chemical_formula_weight         894.29
_chemical_name_systematic
;
[tricarbonyl(1,2-bis{diphenylphosphino}ethane)-2-phenylethynyltungsten)]
;
_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                79.654(2)
_cell_angle_beta                 84.718(2)
_cell_angle_gamma                75.752(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5159(2)
_cell_length_b                   9.9084(2)
_cell_length_c                   18.0985(3)
_cell_measurement_reflns_used    30617
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      34.36
_cell_measurement_theta_min      2.59
_cell_volume                     1625.03(6)
_computing_cell_refinement
;
CrysAlisPro Software, Oxford Diffraction Ltd.,
Version 1.171.33.41
;
_computing_data_collection
;
CrysAlisPro Software, Oxford Diffraction Ltd.,
Version 1.171.33.41
;
_computing_data_reduction
;
CrysAlisPro Software, Oxford Diffraction Ltd.,
Version 1.171.33.41 
;
_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 0.999
_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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            42682
_diffrn_reflns_theta_full        32.58
_diffrn_reflns_theta_max         32.58
_diffrn_reflns_theta_min         2.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.639
_exptl_absorpt_correction_T_max  0.795
_exptl_absorpt_correction_T_min  0.492
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
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            yellow
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.943
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.098
_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     397
_refine_ls_number_reflns         11813
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0194
_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^)+(0.0229P)^2^+0.3034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0446
_refine_ls_wR_factor_ref         0.0452
_reflns_number_gt                10696
_reflns_number_total             11813
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja909764x_si_004.cif
_cod_data_source_block           4
_cod_original_cell_volume        1625.03(5)
_cod_database_code               4102012