Synthesis and Reactivity of the Triply Bonded Binuclear Anion [W2(η5-C5H5)2(μ-PCy2)(μ-CO)2]−: Tungsten Makes a Difference
Alvarez, M. Angeles; García, M. Esther; García-Vivó, Daniel; Ruiz, Miguel A.; Vega, M. Fernanda; Organometallics 29 (2010) 512–; doi:10.1021/om9010005

data_4067529
_publ_section_title
;
 Synthesis and Reactivity of the Triply Bonded Binuclear Anion
 [W2(\h5-C5H5)2(\m-PCy2)(\m-CO)2]&#x2212;: Tungsten Makes a Difference
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              512
_journal_paper_doi               10.1021/om9010005
_journal_volume                  29
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C42 H47 O2 P Sn W2, C H2 Cl2'
_chemical_formula_sum            'C43 H49 Cl2 O2 P Sn W2'
_chemical_formula_weight         1186.08
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                77.1990(10)
_cell_angle_beta                 85.4460(10)
_cell_angle_gamma                68.0370(10)
_cell_formula_units_Z            2
_cell_length_a                   10.16930(10)
_cell_length_b                   11.51920(10)
_cell_length_c                   19.3320(2)
_cell_measurement_reflns_used    7413
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      0.407
_cell_measurement_wavelength     0.71073
_cell_volume                     2048.03(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor, 1997) 
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '90 mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            33508
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    6.413
_exptl_absorpt_correction_T_max  0.28224
_exptl_absorpt_correction_T_min  0.20208
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.401
_refine_diff_density_min         -2.757
_refine_diff_density_rms         0.571
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.276
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.276
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+1.4078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                6867
_reflns_number_total             7409
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9010005_si_002.cif
_cod_data_source_block           compound6
_cod_database_code               4067529