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_4330525
_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            'C42 H37 B Cl2 F4 O P2 S W2'
_chemical_formula_weight         1177.13
_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                 102.70(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.674(4)
_cell_length_b                   13.068(5)
_cell_length_c                   13.067(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     2111.3(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SIEMENS AED'
_diffrn_measurement_method       'teta 2 teta'
_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  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6622
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    5.746
_exptl_absorpt_correction_T_max  0.5442
_exptl_absorpt_correction_T_min  0.1666
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_description       prism
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.728
_refine_diff_density_min         -2.509
_refine_diff_density_rms         0.152
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.006(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         6388
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                5032
_reflns_number_total             6388
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301674k_si_001_1.cif
_cod_data_source_block           compound5
_cod_original_cell_volume        2111.2(13)
_cod_database_code               4330525