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_4102019
_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
' 2(C84 H72 I2 O2 P6 W2), 4(C4 H8 O), C H2 Cl2, 2(F6 P)'
_chemical_formula_sum            'C185 H178 Cl2 F12 I4 O8 P14 W4'
_chemical_formula_weight         4504.72
_chemical_name_systematic
;
[(\m-but-2-yn-1,4-diylidyne)(dicarbonyl)(tri{1,2-bis
(diphenylphosphinoethane)})diiodo-ditungsten)] hexafluorophosphate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 118.139(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.9627(2)
_cell_length_b                   16.7625(2)
_cell_length_c                   36.0870(1)
_cell_measurement_reflns_used    24085
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      32.7018
_cell_measurement_theta_min      2.2580
_cell_volume                     9048.10(18)
_computing_cell_refinement
' CrysAlisPro Software, Oxford Diffraction Ltd., Version 1.171.32'
_computing_data_collection
' CrysAlisPro Software, Oxford Diffraction Ltd., Version 1.171.32'
_computing_data_reduction
' CrysAlisPro Software, Oxford Diffraction Ltd., Version 1.171.32'
_computing_molecular_graphics
; ORTEP-3 for Windows, Version 1.08.
  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 1.70.01.
 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 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type
; Oxford Diffraction (2007). Oxford Diffraction Ltd., 
Xcalibur CCD system
;
_diffrn_measurement_method       'omega and phi 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  0.0725
_diffrn_reflns_av_sigmaI/netI    0.1245
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            96018
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.438
_exptl_absorpt_correction_T_max  0.714
_exptl_absorpt_correction_T_min  0.391
_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.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4424
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_refine_diff_density_max         4.512
_refine_diff_density_min         -1.216
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1048
_refine_ls_number_reflns         27192
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0837P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1621
_reflns_number_gt                13621
_reflns_number_total             27192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja909764x_si_011.cif
_cod_data_source_block           11[PF6]
_cod_original_cell_volume        9048.11(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4102019