Diastereoselective Formation of Complexed Methylenediphosphiranes
Jansen, Helen; Rosenthal, Amos J.; Slootweg, J. Chris; Ehlers, Andreas W.; Lutz, Martin; Spek, Anthony L.; Lammertsma, Koop; Organometallics 27 (2008) 2868–; doi:10.1021/om800188h

data_4071487
_publ_section_title
;
 Diastereoselective Formation of Complexed Methylenediphosphiranes
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2868
_journal_paper_doi               10.1021/om800188h
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C43 H44 O5 P2 W'
_chemical_formula_sum            'C43 H44 O5 P2 W'
_chemical_formula_weight         886.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.009(1)
_cell_angle_beta                 78.960(2)
_cell_angle_gamma                75.101(1)
_cell_formula_units_Z            2
_cell_length_a                   11.3216(4)
_cell_length_b                   13.2755(4)
_cell_length_c                   14.5331(3)
_cell_measurement_reflns_used    40752
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.50
_cell_volume                     1970.75(10)
_computing_cell_refinement       Peakref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            53642
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    3.055
_exptl_absorpt_correction_T_max  0.52
_exptl_absorpt_correction_T_min  0.24
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         8957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0149
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0121P)^2^+0.9628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0317
_refine_ls_wR_factor_ref         0.0324
_reflns_number_gt                8383
_reflns_number_total             8957
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om800188h-file003.cif
_cod_data_source_block           s3832a
_cod_original_cell_volume        1970.74(10)
_cod_database_code               4071487