First Brønsted Acid-Induced Ring Expansion of an Oxaphosphirane Complex: A Combined Experimental and DFT Study
Helten, Holger; Pérez, Janaina Marinas; Daniels, Jörg; Streubel, Rainer; Organometallics 28 (2009) 1221–; doi:10.1021/om8010245

data_4068669
_publ_section_title
;
 First Br\/onsted Acid-Induced Ring Expansion of an Oxaphosphirane
 Complex: A Combined Experimental and DFT Study
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1221
_journal_paper_doi               10.1021/om8010245
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C21 H28 N O6 P Si2 W'
_chemical_formula_weight         661.44
_chemical_name_systematic
;
pentacarbonyl[4-bis(trimethylsilyl)methyl-5-methyl-2-phenyl-
1,3,4-oxazaphosphol-2-ene -&#954;P)Tungsten(0)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2007-12-07T09:56:47-00:00
_audit_creation_method           'manual editing of form.cif'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.5242(2)
_cell_length_b                   17.2471(2)
_cell_length_c                   18.5350(2)
_cell_measurement_reflns_used    61641
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.407
_cell_volume                     5282.37(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.48537E-1
_diffrn_orient_matrix_UB_12      0.98528E-2
_diffrn_orient_matrix_UB_13      -0.308931E-1
_diffrn_orient_matrix_UB_21      0.82531E-2
_diffrn_orient_matrix_UB_22      0.571375E-1
_diffrn_orient_matrix_UB_23      0.54727E-2
_diffrn_orient_matrix_UB_31      0.351914E-1
_diffrn_orient_matrix_UB_32      0.1894E-3
_diffrn_orient_matrix_UB_33      -0.438921E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            93548
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.78
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.559
_exptl_absorpt_correction_T_max  0.6844
_exptl_absorpt_correction_T_min  0.1178
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.82
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.038
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0201
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0449
_refine_ls_wR_factor_ref         0.047
_reflns_number_gt                5087
_reflns_number_total             6047
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om8010245_si_002.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4068669