Novel access to azaphosphiridine complexes and first applications using Brønsted acid-induced ring expansion reactions.
Fankel, Stefan; Helten, Holger; von Frantzius, Gerd; Schnakenburg, Gregor; Daniels, Jörg; Chu, Victoria; Müller, Christina; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 39 (2010) 3472–3481; doi:10.1039/b922166b

data_7024867
_publ_section_title
;
 Novel access to azaphosphiridine complexes and first applications using
 Br\/onsted acid-induced ring expansion reactions.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3472
_journal_page_last               3481
_journal_paper_doi               10.1039/b922166b
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C18 H26 N O5 P S Si2 W'
_chemical_formula_sum            'C18 H26 N O5 P S Si2 W'
_chemical_formula_weight         639.46
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                72.925(3)
_cell_angle_beta                 75.155(3)
_cell_angle_gamma                77.227(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3006(4)
_cell_length_b                   9.8061(4)
_cell_length_c                   15.3241(6)
_cell_measurement_reflns_used    10736
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      2.20
_cell_volume                     1275.21(9)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_details      ' 170 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10310
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.20
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           45
_diffrn_source_power             2.25
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.794
_exptl_absorpt_correction_T_max  0.6961
_exptl_absorpt_correction_T_min  0.4876
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.197
_refine_diff_density_min         -1.250
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       0.0099(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5790
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0851
_reflns_number_gt                5162
_reflns_number_total             5790
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b922166b.txt
_cod_data_source_block           greg607
_cod_database_code               7024867