Ferrocenium salt induced ring expansion of a 2H-azaphosphirene complex: Synthesis of the first Δ3-1,4,2-oxazaphospholene complexes †
Streubel, Rainer; Neumann, Christoph; Jones, Peter G.; Journal of the Chemical Society, Dalton Transactions  (2000) 2495–; doi:10.1039/b004795n

data_7009960
_publ_section_title
;
 Ferrocenium salt induced ring expansion of a 2H-azaphosphirene
 complex: Synthesis of the first \D3-1,4,2-oxazaphospholene
 complexes&#x200A;&#x2020;
;
_journal_issue                   15
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2495
_journal_paper_doi               10.1039/b004795n
_journal_year                    2000
_chemical_formula_sum            'C27.5 H40 N O6 P Si2 W'
_chemical_formula_weight         751.60
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.330(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.058(4)
_cell_length_b                   10.4819(12)
_cell_length_c                   19.602(2)
_cell_measurement_reflns_used    5841
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     6459.0(13)
_computing_cell_refinement       'Bruker Saint'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       '\w- & \f-scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38692
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    3.739
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.479
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         9462
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+0.3653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0589
_reflns_number_gt                7298
_reflns_number_total             9462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004795n.txt
_cod_data_source_block           neuma
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (65
times).

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (38 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        6458.9(13)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C27.50 H40 N O6 P Si2 W'
_cod_database_code               7009960