Transformation between Diphosphinoamines and Iminobiphosphines: a Reversible PNP \λeftarrow→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_4310828
_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         'C53 H44 N3 P4, B F4, 2(C H2 Cl2)'
_chemical_formula_sum            'C55 H48 B Cl4 F4 N3 P4'
_chemical_formula_weight         1103.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_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                   19.359(4)
_cell_length_b                   19.501(4)
_cell_length_c                   14.1785(18)
_cell_measurement_reflns_used    2718
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      19.1366
_cell_measurement_theta_min      1.7228
_cell_volume                     5352.7(17)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32516
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    0.395
_exptl_absorpt_correction_T_max  0.5770
_exptl_absorpt_correction_T_min  0.1110
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
; 
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0006(5)
_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   1.176
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         4728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0941P)^2^+1.0732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1772
_reflns_number_gt                3414
_reflns_number_total             4728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049850wsi20040216_044808_2.cif
_cod_data_source_block           2BF4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 
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_cod_database_code               4310828