Comparison of H-H versus Si-H σ-Bond Coordination and Activation on 16e Metal Fragments. Organosilane, N2, and Ethylene Addition to the Agostic Complex W(CO)3(PR3)2 and Dynamic NMR Behavior of the Latter
Matthew D. Butts; Jeffrey C. Bryan; Xiao-Liang Luo; Gregory J. Kubas; Inorganic Chemistry 36 (1997) 3341–3353; doi:10.1021/ic960870a

data_4323497
_publ_section_title
;
 Comparison of H-H versus Si-H \s-Bond Coordination and Activation on 16e
 Metal Fragments. Organosilane, N2, and Ethylene Addition to the Agostic
 Complex W(CO)3(PR3)2 and Dynamic NMR Behavior of the Latter
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3341
_journal_page_last               3353
_journal_paper_doi               10.1021/ic960870a
_journal_volume                  36
_journal_year                    1997
_chemical_formula_moiety         'W, 3(C O), 2(C18 H33 P), (C2 H4)'
_chemical_formula_sum            'C41 H70 O3 P2 W'
_chemical_formula_weight         856.76
_chemical_name_common
;
trans, mer bis(tricyclohexanophosphine)tricarbonylethylenetungsten
;
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                87.01(4)
_cell_angle_beta                 81.03(3)
_cell_angle_gamma                74.04(3)
_cell_formula_units_Z            2
_cell_length_a                   11.250(5)
_cell_length_b                   12.716(6)
_cell_length_c                   14.458(6)
_cell_measurement_temperature    203(2)
_cell_volume                     1964.2(15)
_computing_data_reduction        SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       \q/2\q
_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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7339
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.42
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.058
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       cube
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.090
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.066
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         6954
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.065
_refine_ls_restrained_S_obs      1.077
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_obs          0.0289
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+0.7416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0610
_refine_ls_wR_factor_obs         0.0576
_reflns_number_observed          6105
_reflns_number_total             6954
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960870a_2.cif
_cod_data_source_block           wet
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+0.7416P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+0.7416P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323497