Transformation between Diphosphinoamines and Iminobiphosphines: a Reversible PNP ←→ NP-P Rearrangement Triggered by Protonation/Deprotonation
Zhaofu Fei; Nermin Biricik; Dongbin Zhao; Rosario Scopelliti; Paul J. Dyson; Inorganic Chemistry 43 (2004) 2228–2230; doi:10.1021/ic049850w

data_4310827
_publ_contact_author_address
;
Institut de Chimie Mol\'eculaire et Biologique
\'Ecole Polytechnique F\'ed\'erale de Lausanne
1015 Lausanne
Switzerland
;
_publ_contact_author_email       paul.dyson@epfl.ch
_publ_contact_author_fax         '+41 21 693 9885'
_publ_contact_author_name        'Paul J. Dyson'
_publ_contact_author_phone       '+41 21 693 9854'
_publ_section_title
;
 Transformation between Diphosphinoamines and Iminobiphosphines: a
 Reversible PNP \\leftarrow\\rightarrow NP-P Rearrangement Triggered by
 Protonation/Deprotonation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2228
_journal_page_last               2230
_journal_paper_doi               10.1021/ic049850w
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C29 H25 N2 P2, B F4'
_chemical_formula_sum            'C29 H25 B F4 N2 P2'
_chemical_formula_weight         550.26
_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                96.71(5)
_cell_angle_beta                 102.60(4)
_cell_angle_gamma                102.69(4)
_cell_formula_units_Z            2
_cell_length_a                   9.893(4)
_cell_length_b                   11.133(7)
_cell_length_c                   12.673(6)
_cell_measurement_reflns_used    753
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      16.92115
_cell_measurement_theta_min      1.67535
_cell_volume                     1308.8(12)
_computing_cell_refinement       'Oxford Diffraction CrysAlis RED'
_computing_data_collection       'marresearch mar345'
_computing_data_reduction        'Oxford Diffraction CrysAlis RED'
_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      140(2)
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'marresearch mar345 IPDS'
_diffrn_measurement_method
'60 images with deltaphi = 3 deg. and exp. time = 180 sec.'
_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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8502
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  0.6170
_exptl_absorpt_correction_T_min  0.1440
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
; 
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.006(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1073P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1687
_refine_ls_wR_factor_ref         0.1951
_reflns_number_gt                2553
_reflns_number_total             4327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049850wsi20040216_044808_1.cif
_cod_data_source_block           8BF4(supplementary_structure)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1308.9(12)
_cod_database_code               4310827