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_4068670
_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            'C26 H30 N O6 P Si2 W'
_chemical_formula_weight         723.51
_chemical_name_systematic
;
pentacarbonyl(4-bis(trimethylsilyl)methyl-2,5-diphenyl-
1,3,4-oxazaphosphol-2-ene
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of form.cif'
_cell_angle_alpha                90
_cell_angle_beta                 109.4830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3301(5)
_cell_length_b                   11.3528(2)
_cell_length_c                   17.6200(5)
_cell_measurement_reflns_used    12880
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2890.99(14)
_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 0.98
_diffrn_measured_fraction_theta_max 0.98
_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      0.474495E-1
_diffrn_orient_matrix_UB_12      -0.517228E-1
_diffrn_orient_matrix_UB_13      0.381769E-1
_diffrn_orient_matrix_UB_21      0.315309E-1
_diffrn_orient_matrix_UB_22      0.710921E-1
_diffrn_orient_matrix_UB_23      0.304565E-1
_diffrn_orient_matrix_UB_31      -0.392698E-1
_diffrn_orient_matrix_UB_32      -0.54145E-2
_diffrn_orient_matrix_UB_33      0.352018E-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  0.0415
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20829
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.8
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.173
_exptl_absorpt_correction_T_max  0.6589
_exptl_absorpt_correction_T_min  0.2197
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.108
_refine_diff_density_min         -3.105
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.99
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         6510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.99
_refine_ls_R_factor_all          0.035
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0647
_reflns_number_gt                5592
_reflns_number_total             6510
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8010245_si_002.cif
_cod_data_source_block           global
_cod_original_cell_volume        2890.99(13)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4068670