Reactions of the Unsaturated Hydroxo Complex [W2Cp2(OH)(μ-PPh2)2(CO)]BF4 with Mono- and Bidentate Ligands Having E-H bonds (E = O, S, N)
Fernanda Cimadevilla; M. Esther García; Daniel García-Vivó; Miguel A. Ruiz; Claudia Graiff; Antonio Tiripicchio; Inorganic Chemistry 51 (2012) 10427–10436; doi:10.1021/ic301674k

data_4330526
_publ_section_title
;
 Reactions of the Unsaturated Hydroxo Complex [W2Cp2(OH)(\m-PPh2)2(CO)]BF4
 with Mono- and Bidentate Ligands Having E-H bonds (E = O, S, N)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10427
_journal_page_last               10436
_journal_paper_doi               10.1021/ic301674k
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C83 H70 Cl2 O6 P4 W4'
_chemical_formula_weight         2093.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.31(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.553(5)
_cell_length_b                   18.183(4)
_cell_length_c                   19.853(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      8
_cell_volume                     3769(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.1109
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11570
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    6.292
_exptl_absorpt_correction_T_max  0.4755
_exptl_absorpt_correction_T_min  0.1405
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_description       prism
_exptl_crystal_F_000             2012
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.134
_refine_diff_density_min         -1.547
_refine_diff_density_rms         0.174
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         11297
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1088
_reflns_number_gt                6903
_reflns_number_total             11297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301674k_si_001_2.cif
_cod_data_source_block           compound14
_cod_database_code               4330526