The azaphosphiridine to terminal phosphinidene complex rearrangement ‒ looking for non-covalent interactions of a highly reactive species
Jose Manuel Villalba Franco; Arturo Espinosa Ferao; Gregor Schnakenburg; Rainer Streubel; Chem.Commun. 49 (2013) 9648–; doi:10.1039/c3cc45477k

data_7109857
_publ_section_title
;
 The azaphosphiridine to terminal phosphinidene complex rearrangement --
 looking for non-covalent interactions of a highly reactive species
;
_journal_name_full               Chem.Commun.
_journal_page_first              9648
_journal_paper_doi               10.1039/c3cc45477k
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C21 H22 N O6 P W'
_chemical_formula_sum            'C21 H22 N O6 P W'
_chemical_formula_weight         599.22
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.595(2)
_cell_angle_beta                 78.246(2)
_cell_angle_gamma                66.290(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8600(4)
_cell_length_b                   10.8854(5)
_cell_length_c                   12.8306(5)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.15
_cell_measurement_theta_min      2.56
_cell_volume                     1108.89(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       '\f and \w CCD rotation images, thin slices'
_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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13781
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         3.24
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.317
_exptl_absorpt_correction_T_max  0.3386
_exptl_absorpt_correction_T_min  0.1763
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs 2008/2'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5338
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0174
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0093P)^2^+0.9685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0404
_refine_ls_wR_factor_ref         0.0410
_reflns_number_gt                5130
_reflns_number_total             5338
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            c3cc45477k.txt
_cod_data_source_block           greg1752f
_cod_original_cell_volume        1108.89(8)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_database_code               7109857