Electrocyclization of Phosphahexatrienes: An Approach to λ5-Phosphinines
Yurii V. Svyaschenko; Bogdan B. Barnych; Dmitriy M. Volochnyuk; Nadiya V. Shevchuk; Aleksandr N. Kostyuk; Journal of Organic Chemistry 76 (2011) 6125–6133; doi:10.1021/jo200847r

data_4026483
_publ_section_title
;
 Electrocyclization of Phosphahexatrienes: An Approach to \l5-Phosphinines
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6125
_journal_page_last               6133
_journal_paper_doi               10.1021/jo200847r
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C13 H22 N2 O2 P'
_chemical_formula_sum            'C13 H22 N2 O2 P'
_chemical_formula_weight         269.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.65380(10)
_cell_length_b                   11.5537(2)
_cell_length_c                   15.5946(3)
_cell_measurement_reflns_used    8539
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.53
_cell_measurement_theta_min      2.61
_cell_volume                     1379.03(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14886
_diffrn_reflns_theta_full        28.59
_diffrn_reflns_theta_max         28.59
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.9618
_exptl_absorpt_correction_T_min  0.9291
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_meas      0
_exptl_crystal_description       prizm
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+0.1279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0722
_reflns_number_gt                3124
_reflns_number_total             3301
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo200847r_si_001.cif
_cod_data_source_block           e:\x-ray\2011\svjach\svasch1\sv1
_cod_database_code               4026483