Metallation-induced migration of phosphorus from nitrogen to carbon in 1-oxo-2,8-diphenyl-2,5,8-triaza-1λ5-phosphabicyclo[3.3.0]octane: unusual bonding parameters of the double migration product
He, Zhengjie; Modro, Tomasz A.; Van Rooyen, Petrus H.; Bourne, Susan A.; Chemical Communications  (1999) 853–; doi:10.1039/a901877h

data_7110525
_publ_section_title
;
 Metallation-induced migration of phosphorus from nitrogen to carbon in
 1-oxo-2,8-diphenyl-2,5,8-triaza-1\l5-phosphabicyclo[3.3.0]octane: unusual
 bonding parameters of the double migration product
;
_journal_issue                   9
_journal_name_full               'Chemical Communications'
_journal_page_first              853
_journal_paper_doi               10.1039/a901877h
_journal_year                    1999
_chemical_formula_sum            'C16 H18 N3 O P'
_chemical_formula_weight         299.30
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.648(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.201(3)
_cell_length_b                   9.0538(16)
_cell_length_c                   20.266(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      16.96
_cell_measurement_theta_min      14.17
_cell_volume                     1504.1(6)
_computing_cell_refinement       'Enraf Nonius CAD4'
_computing_data_collection       'Enraf Nonius CAD4'
_computing_data_reduction        'Enraf Nonius CAD4'
_computing_molecular_graphics    Ortep
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       omega-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            4659
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        2.0
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_T_max  0.9710
_exptl_absorpt_correction_T_min  0.9050
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         4380
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0776
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+0.8458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.1980
_reflns_number_gt                2899
_reflns_number_total             4380
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            901877hsup1.cif
_cod_data_source_block           compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+0.8458P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+0.8458P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1504.2(7)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7110525