Regio- and Stereochemical Aspects of the Substitution Reaction between the Molybdenocene and Tungstenocene Dichlorides (η5-C5H4-R)2MCl2(R = CMe3, SiMe3; M = Mo, W) and Metallophosphide Anions [(CO)5M‘PPh2]Li (M‘ = Mo, W)
Comte, Virginie; Blacque, Olivier; Kubicki, Marek M.; Moïse, Claude; Organometallics 20 (2001) 5432–; doi:10.1021/om010495g

data_4077390
_publ_section_title
;
 Regio- and Stereochemical Aspects of the Substitution Reaction between
 the Molybdenocene and Tungstenocene Dichlorides (\h5-C5H4-R)2MCl2(R =
 CMe3, SiMe3; M = Mo, W) and Metallophosphide Anions
 [(CO)5M&#x2018;PPh2]Li (M&#x2018; = Mo, W)
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5432
_journal_paper_doi               10.1021/om010495g
_journal_volume                  20
_journal_year                    2001
_chemical_formula_moiety         'C33 H36 Cl O5 P Si2 W2'
_chemical_formula_sum            'C34.5 H39 Cl O5.5 P Si2 W2'
_chemical_formula_weight         1032.97
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                85.825(10)
_cell_angle_beta                 71.238(9)
_cell_angle_gamma                64.854(9)
_cell_formula_units_Z            4
_cell_length_a                   15.6852(17)
_cell_length_b                   16.668(2)
_cell_length_c                   17.305(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.25
_cell_volume                     3867.1(9)
_computing_cell_refinement       'CAD4 EXPRESS'
_computing_data_collection       'CAD4 EXPRESS'
_computing_data_reduction        'XCAD4 (Harms, 1996)'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       Omega-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16265
_diffrn_reflns_theta_full        26.33
_diffrn_reflns_theta_max         26.33
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        33
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.155
_exptl_absorpt_correction_T_max  0.9990
_exptl_absorpt_correction_T_min  0.7026
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         15666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0391P)^2^+5.1406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0890
_reflns_number_gt                11258
_reflns_number_total             15666
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010495g.cif
_cod_data_source_block           2b-SiW
_cod_original_cell_volume        3867.1(8)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C34.50 H39 Cl O5.50 P Si2 W2'
_cod_database_code               4077390