Chemistry of the Oxophosphinidene Ligand. 1. Electronic Structure of the Anionic Complexes [MCp{P(O)R*}(CO)2]- (M = Mo, W; R* = 2,4,6-C6H2tBu3) and Their Reactions with H+ and C-Based Electrophiles.
María Alonso; M. Angeles Alvarez; M. Esther García; Daniel García-Vivó; Miguel A. Ruiz; Inorganic Chemistry 49 (2010) 8962–8976; doi:10.1021/ic101261f

data_4316623
_publ_section_title
;
 Chemistry of the Oxophosphinidene Ligand. 1. Electronic Structure of the
 Anionic Complexes [MCp{P(O)R*}(CO)2]- (M = Mo, W; R* = 2,4,6-C6H2tBu3)
 and Their Reactions with H+ and C-Based Electrophiles.
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8962
_journal_page_last               8976
_journal_paper_doi               10.1021/ic101261f
_journal_volume                  49
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C25 H36 Cl1 O3 P1 W1'
_chemical_formula_sum            'C25 H36 Cl O3 P W'
_chemical_formula_weight         634.81
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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      2.2
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.019(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.021(6)
_cell_length_b                   11.003(3)
_cell_length_c                   12.516(4)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      27.125
_cell_measurement_theta_min      2.685
_cell_measurement_wavelength     0.71073
_cell_volume                     2619.4(14)
_computing_cell_refinement       'Brucker Smart'
_computing_data_collection       'Brucker Smart'
_computing_data_reduction        'Brucker Smart'
_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      120.0(1)
_diffrn_measured_fraction_theta_full 0.849
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_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  0.0874
_diffrn_reflns_av_unetI/netI     0.1014
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24499
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.18
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    4.596
_exptl_absorpt_correction_T_max  0.8375
_exptl_absorpt_correction_T_min  0.2608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER Sadabs'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.61
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.37
_refine_diff_density_min         -3.456
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         5083
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.052
_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^)+(0.0715P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.12
_refine_ls_wR_factor_ref         0.1321
_reflns_number_gt                3501
_reflns_number_total             5083
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101261f_si_002_3.cif
_cod_data_source_block           comp7
_cod_database_code               4316623