Going for strain: synthesis of the first 3-imino-azaphosphiridine complexes and their conversion into oxaphosphirane complex valence isomers
Jose Manuel Villalba Franco; Takahiro Sasamori; Gregor Schnakenburg; Arturo Espinosa Ferao; Rainer Streubel; Chem.Commun. 51 (2015) 3878–; doi:10.1039/C4cc10266E

data_7116588
_publ_section_title
;
 Going for strain: synthesis of the first 3-imino-azaphosphiridine
 complexes and their conversion into oxaphosphirane complex valence
 isomers
;
_journal_name_full               Chem.Commun.
_journal_page_first              3878
_journal_paper_doi               10.1039/C4cc10266E
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C22 H29 N2 O5 P W'
_chemical_formula_sum            'C22 H29 N2 O5 P W'
_chemical_formula_weight         616.29
_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
_audit_update_record
;
2014-12-15 deposited with the CCDC.
2015-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                108.084(4)
_cell_angle_beta                 95.194(4)
_cell_angle_gamma                118.186(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9909(5)
_cell_length_b                   11.0605(6)
_cell_length_c                   12.8740(10)
_cell_measurement_reflns_used    5171
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.22
_cell_measurement_theta_min      2.38
_cell_volume                     1257.68(15)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_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            12812
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         3.16
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.688
_exptl_absorpt_correction_T_max  0.9121
_exptl_absorpt_correction_T_min  0.3753
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs 2008/2'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.699
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         6035
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+5.0322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                5137
_reflns_number_total             6035
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc10266e2.cif
_cod_data_source_block           3299f
_cod_database_code               7116588